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    《化學試劑》2022年第8期中英文摘要(附整期文章PDF文檔)

    敞開式離子化質譜技術在中藥材中藥飲片質量評價中的應用進展

     

    黃文靜1,2,葉楚璇1,3,徐浩然1,4,黃志偉1,3,王登輝1,王樂琪1,3,李莎莎*1,2,3,嚴詩楷1,2,3,4,肖雪*1,2

    1. 廣東藥科大學 中醫藥研究院 中藥學院 廣東省代謝病中西醫結合研究中心,廣東 廣州  510006;

    2. 國家藥品監督管理局藥品快速檢驗技術重點實驗室(廣東省藥品檢驗所),廣東 廣州  510663;

    3. 廣州中醫藥大學第二附屬醫院,廣東 廣州  510120;4. 上海交通大學 藥學院,上海  200240

     

    摘要:中藥材及中藥飲片是中藥產業鏈的重要組成部分,其質量是保障中成藥質量和穩定發揮臨床療效的基礎。為了實現中藥材及中藥飲片質量更高效的控制與監管,新技術、新設備、新方法不斷產生。敞開式離子化質譜技術是近些年迅速發展起來的一種新型檢測技術,具有實時、直接、準確、快速的特有優點,在中藥分析、質量分析與質量控制領域的應用越來越多,取得了良好的應用效果。歸納梳理了敞開式離子化質譜技術的基本原理、特點,其在中藥材及中藥飲片質量分析與評價中的應用現狀,總結該技術在中藥材及中藥飲片質量評價中所面臨的問題,并對其未來發展方向進行展望。

    關鍵詞:敞開式離子化;質譜;中藥材;中藥飲片;質量控制

    中圖分類號:R917     文獻標識碼:A            文獻編號:0258-32832022

     

    Application Progress in Quality Evaluation of Chinese Medicinal Materials and Chinese Medicine Decoction Pieces based on Ambient Ionization Mass Spectrometry HUANG Wen-jing1,2, YE Chu-xuan1,3, XU Hao-ran1,4, HUANG Zhi-wei1,3, WANG Deng-hui1, Wang Le-qi1,3, LI Sha-sha*1,2,3, YAN Shi-kai1,2,3,4, XIAO Xue*1,2 (1. Institute of Traditional Chinese Medicine, School of Traditional Chinese Medicine, Guangdong Metabolic Disease Research Center of Integrated Chinese and Western Medicine, Guangdong Pharmaceutical University, Guangzhou 510006; 2. NMPA Key Laboratory for Rapid Testing Technology of Drugs, Guangdong Institute for Drug Control, Guangzhou 510663; 3. The Second Affiliated Hospital of Guangzhou University of Chinese Medicine, Guangzhou 510120; 4. School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China), Huaxue Shiji, 2022, 44(8),

    Abstract: Chinese medicinal materials and Chinese medicinal decoction pieces are the important parts of the Chinese medicine industry chain, and the quality is the basis of guaranteeing the quality of Chinese patent medicine and developing its clinical efficacy stably. To effectively supervise the quality of Chinese medicinal materials and decoction pieces, new techniques, advanced instruments and new methods for quality control have been developed. Ambient ionization mass spectrometry (AIMS) is a new detection technology developed rapidly in recent years. AIMS has the unique advantages of being real-time, direct, accurate, and fast. In recent years, AIMS has been applied in this field. In this paper, the basic principle, characteristics, and application progress of AIMS in quality evaluation of Chinese herbal decoction pieces were summarized, the problems faced by this technology in quality evaluation of Chinese herbal decoction pieces were summarized and the future development direction of this technology has prospected.

    Key wordsambient ionization; mass spectrometry; Chinese medicinal materials; Chinese herbal medicine; quality control

    引用本文:黃文靜, 葉楚璇, 徐浩然, .敞開式離子化質譜技術在中藥材及中藥飲片質量評價中的應用進展[J]. 化學試劑, 2022, 448):1079-1087.

     

     

    植物乳桿菌發酵黑果枸杞的代謝組學研究

    李麗1,馮華峰*2,周淳3,胡坪1,章弘揚*1

    1. 華東理工大學 化學與分子工程學院,上海市功能性材料化學重點實驗室,上海  200237;2. 上海商學院 食品系,上海  200235;3. 上海甘泓生物醫學科技有限公司,上海  200131)

    摘要以植物乳桿菌GH-6發酵黑果枸杞漿為研究對象,分析發酵前后黑果枸杞漿中差異性代謝物的含量變化。采用超高效液相色譜-靜電場軌道肼質譜聯用(UPLC-Orbitrap MS)技術,首先對發酵前后黑果枸杞漿的成分進行分析,共鑒定出61個代謝物。隨后,在原漿、發酵液以及添加蔗糖及乳清蛋白后的發酵液中篩選出22個差異性代謝物,其中4種花青素類、3種有機酸類、2種糖類、3種氨基酸類、7種小肽類和3種嘌呤類。結果表明,由于植物乳桿菌GH-6糖苷酶的水解作用,促使花青素類及糖類物質的含量上升;經發酵引起的乳酸生成增加,可有效調節黑果枸杞發酵液的風味;益生乳酸菌具有的肽轉運系統使得二肽、三肽類物質水解,天冬氨酸-異亮氨酸、纈氨酰-谷氨酸及纈氨酰-纈氨酰-纈氨酸在發酵后未被檢出,說明這三種肽類可能優先被植物乳桿菌GH-6所利用。此外,植物乳桿菌GH-6還具有降解嘌呤的能力,致使發酵液中嘌呤類物質的含量降低??傊?,通過植物乳桿菌GH-6發酵能顯著影響黑果枸杞漿中的代謝變化,本研究將為黑果枸杞有效營養成分的開發利用以及發酵制品等相關產品的研發提供參考和新的應用方向。

    關鍵詞黑果枸杞;植物乳桿菌GH-6;發酵;代謝組學;多元變量統計分析

    中圖分類號:O65    文獻標識碼:A    文章編號:0258-32832022--

     

    Metabolomics study of Lactobacillus Plantarum Fermented Lycium Ruthenicum Murr. Li Li1, Huafeng Feng*2, Chun Zhou3, Ping Hu1, Hongyang Zhang*1 (1. Shanghai Key Laboratory of Functional Materials Chemistry, School of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai 200237, China; 2. The Department of Food, Shanghai Business School, Shanghai 200235, China; 3. Shanghai Ganhong Biomedical Technology Co., Ltd., Shanghai 200131, China), Huaxue Shiji, 44(8),

    AbstractTaking lactobacillus plantarum GH-6 fermented Lycium Ruthenicum Murr. as the research object, the content changes of differential metabolites in Lycium Ruthenicum Murr. before and after fermentation was analyzed. By using ultra-high-performance liquid chromatography-orbitrap mass spectrometry (UPLC-Orbitrap MS), the composition of Lycium Ruthenicum Murr. before and after fermentation was analyzed, and a total of 61 metabolites were identified. After then, 22 differential metabolites were screened in the puree, fermentation broth, and fermentation broth after adding sucrose and whey protein, including 4 anthocyanins, 3 organic acids, 2 carbohydrates, and 3 amino acids, 7 small peptides, and 3 purines. The results demonstrated that due to the hydrolysis of lactobacillus plantarum GH-6 glycosidase, the content of anthocyanins and sugars increased. The increment of lactic acid induced by fermentation could effectively adjust the flavor of the fermentation broth of Lycium Ruthenicum Murr. The peptide transport system of probiotic lactic acid bacteria could hydrolyze dipeptide and tripeptide compounds, and Asp-Ile, Val-Glu, and Val-Val-Val were not detected after fermentation, indicating that these peptides might be preferentially utilized by lactobacillus Plantarum GH-6. In addition, lactobacillus plantarum GH-6 can degrade purines, which reduces the content of purines in the fermentation broth. In conclusion, the fermentation of Lactobacillus plantarum GH-6 can significantly affect the metabolic alterations in Lycium Ruthenicum Murr., and this study can provide a reference and novel application directions for the development and utilization of effective nutritional components of Lycium Ruthenicum Murr., as well as the research and development of its fermented products and other related products.

    Key wordsLycium Ruthenicum Murr.; lactobacillus plantarum GH-6; fermentation; metabolomics; multivariate statistical analysis

    引用本文李麗,馮華峰,周淳,等. 植物乳桿菌發酵黑果枸杞的代謝組學研究[J]. 化學試劑,2022, 4481088-1096.

     

    基于中藥Q-marker理論的經典名方枳實薤白桂枝湯關鍵成分發現與量質傳遞研究

    李明潺1,楊紅素2,徐家山2,曲珍妮3,段宏泉3,董林毅*3,孫露*4

    (1. 天津醫科大學總醫院,天津 300052;2. 通化玉圣藥業有限公司,吉林 通化 134000;3. 天津醫科大學 藥學院,天津 300070;4. 天津醫科大學 朱憲彝紀念醫院 天津市內分泌研究所 國家衛健委激素與發育重點實驗室 天津市代謝性疾病重點實驗室,天津 300134)

    摘要:枳實薤白桂枝湯收錄于國家經典名方目錄,中藥質量標志物(Q-marker)理論有助于方劑中關鍵成分的發現與量質傳遞研究。采用液質聯用技術指認枳實薤白桂枝湯中的Q-marker,進行指紋圖譜方法學考察和相似度分析,計算方劑出膏率和關鍵成分的含量轉移率。最終指認大麥芽堿、麥角甾苷、新北美圣草苷、蕓香柚皮苷、柚皮苷、橙皮苷、新橙皮苷、異米拉素、苜蓿素、和厚樸酚和厚樸酚為枳實薤白桂枝湯Q-marker,18批樣品指紋圖譜相似度分析結果均大于0.92,平均出膏率為17.06%,關鍵成分的轉移率以腺苷、辛弗林、桂皮醛、厚樸酚、和厚樸酚計算分別為87.49%、79.95%、25.04%、6.18%、8.80%。本實驗確定了枳實薤白桂枝湯質量標志物,結合指紋圖譜及關鍵成分的量質傳遞研究,為枳實薤白桂枝湯質量評價提供了依據。

    關鍵詞:枳實薤白桂枝湯;液質聯用;中藥指紋圖譜;中藥質量標志物;經典名方

    中圖分類號:R286.02    文獻標識碼:A    文章編號:0258-32832022--

     

    Study on the discovery of the index components and quantitative-qualitative transfer of Classical prescription Zhishi Xiebai Guizhi Decoction based on Q-marker LI Ming-chan1, YANG Hong-su2, XU Jia-shan2, QU Zhen-ni3, DUAN Hon-quan3,DONG Lin-yi*3,SUN Lu*4(1.General Hospital, Tianjin Medical University, Tianjin 300052, China; 2. Tonghua Yu Sheng Pharmaceutical Co., Ltd., Tonghua 134000, China; 3. College of Pharmacy, Tianjin Medical University, Tianjin 300070, China; 4. NHC Key Laboratory of Hormones and Development/Tianjin Key Laboratory of Metabolic Diseases, Chu Hsien-IMemorial Hospital/Tianjin Institute of Endocrinology, Tianjin Medical University, TIANJIN 300134, China), Huaxue Shiji, 44(8),

    AbstractZhishi Xiebai Guizhi Decoction was included in the catalog of national classic prescriptions. Q-marker theory was helpful in the discovery of the index components and quantitative-qualitative transfer study in Chinese herbal prescriptions. Q-marker in Zhishi Xiebai Guizhi Decoction was identified by LC-MS and the fingerprint methodology was investigated, and the similarity analysis was evaluated. The paste-forming rate and the transfer rate of index components were also calculated. Q-marker were identified as follows: Hordenine, Verbascoside, Neoeriocitrin, Narirutin, Naringin, Hesperidin, Neohesperidin, Isoramil, Tricin, Honokiol, Magnolol. The similarity of 18 batches of Zhishi Xiebai Guizhi Decoction samples was more than 0.92. The average paste-forming rate was 17.06%. The transfer rates of adenosine, synephrine, cinnamaldehyde, honokiol, and honokiol were 87.49%, 79.95%, 25.04%, 6.18%, and 8.80%, respectively. In this study, the Q-markers of Zhishi Xiebai Guizhi Decoction were determined. Combined with the fingerprint and the quantitative-qualitative transfer of index components, it provided a basis for the quality evaluation of classical prescription Zhishi Xiebai Guizhi Decoction.

    Key wordsZhishi Xiebai Guizhi decoction; LC-MS; fingerprints; Q-marker;classical prescription

    引用本文李明潺,楊紅素,徐家山,等. 基于中藥Q-marker理論的經典名方枳實薤白桂枝湯關鍵成分發現與量質傳遞研究[J]. 化學試劑,2022,448:1097-1102.

     

     

    2D-LC在中藥分析與質量控制中的應用進展

    葉楚璇1,3,黃文靜1,2,覃思意1,麥子盈1,4,王樂琪1,3,李莎莎*1,2,3,徐浩然1,王登輝1,嚴詩楷1,3,4,肖雪*1,2

    1. 廣東藥科大學 中醫藥研究院 廣東省代謝病中西醫結合研究中心,廣東 廣州  510006;2. 國家藥品監督管理局 藥品快速檢驗技術重點實驗室(廣東省藥品檢驗所),廣東 廣州  510663;3. 廣州中醫藥大學 第二附屬醫院,廣東 廣州  510120;4. 上海交通大學 藥學院,上海  200240

    摘要:中藥質量控制是保證其藥效及安全的關鍵因素,也是中醫藥產業良性發展的重要保障。高效液相色譜技術作為一種經典、高效的檢測技術,具有強大的分離效能,能夠對中藥中復雜成分進行有效分離及含量測定,已廣泛應用于中藥的質量控制中。隨著液相技術的發展,二維液相色譜技術的出現彌補了一維液相色譜技術中樣品前處理復雜,基體干擾較大等缺點,其靈敏度更高,分離度更好,能夠快速,準確對中藥做出分析、評價及質量控制。二維液相色譜技術因其普適性與簡便性,使得中藥分析更加全面、更加完善。本文從二維液相色譜技術在中藥化學成分的系統分離、全面定性、精準定量、風險物質檢測等多個方面,闡述二維液相色譜技術在中藥分析及質量控制中發揮的作用。

    關鍵詞:二維液相;中藥分析;質量控制;應用進展

    中圖分類號      文獻標識碼A       文章編號0258-32832022--

     

    Application Progress of 2D-LC in Analysis and Quality Control of Traditional Chinese Medicine YE Chu-xuan1,3, HUANG Wen-jing1,2, QIN Si-yi1, Mai Zi-ying1,4, Wang Le-qi1,3, LI Sha-sha*1,2,3, XU Hao-ran1, WANG Deng-hui1, YAN Shi-kai1,3,4, XIAO Xue*1,2 (1. Institute of Traditional Chinese Medicine, Guangdong Metabolic Disease Research Center of Integrated Chinese and Western Medicine, Guangdong Pharmaceutical University, Guangzhou 510006, China; 2. NMPA Key Laboratory for Rapid Testing Technology of Drugs, Guangdong Institute for Drug Control, Guangzhou 510663, China; 3. The Second Affiliated Hospital of Guangzhou University of Chinese Medicine, Guangzhou 510120, China; 4. School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China), Huaxue Shiji, 44(8),

    AbstractQuality control of Traditional Chinese medicine is the key factor to ensuring its efficacy and safety, and also an important guarantee for the continuous development of the Traditional Chinese medicine industry. As a classic and efficient detection technology, high-performance liquid chromatography (HPLC) has been widely used in the quality control of Traditional Chinese medicine because of its powerful separation skills and effective separation and content determination of complex components in Traditional Chinese medicine. With the development of liquid phase technology, the appearance of two-dimensional liquid chromatography technology (2D-LC) has made up for the shortcomings of one-dimensional liquid chromatography technology, such as complex sample pretreatment, large matrix interference, and so on. Its sensitivity is higher, the separation degree is better, and it can quickly and accurately evaluate and control the quality of Traditional Chinese medicine. Due to its universality and simplicity, 2D-LC makes qualitative and quantitative analysis of TCM more comprehensive. This paper aims to expound on the role of 2D-LC in the analysis and quality control of Traditional Chinese medicine from the following aspects, such as the overall characterization, the study of chemical composition, the quantitative analysis of complex components, and the control and control of risk substances, etc.

    Key wordstwo-dimensional liquid chromatography; analysis of traditional Chinese medicine; quality control; Application progress

    引用本文葉楚璇,黃文靜,覃思意,等. 2D-LC在中藥分析與質量控制中的應用進展[J]. 化學試劑,2022, 4481103-1110.

     

     

    小葉黃楊化學成分及心肌細胞保護作用研究

    王瑞1,張巖1,MUHAMMAD Ishaq1,田艷2,付登林2,郁華軍*2,肖雪3,嚴詩楷1,2,3,金慧子*1

    (1.上海交通大學 藥學院,上海  200240; 2.貴州景誠制藥有限公司,貴州  貴陽 550200;

    3.廣東藥科大學 中醫藥研究院,廣東  廣州 510006)

    摘要:研究小葉黃楊(Buxus sinica var. parvifolia M. Cheng)葉子的化學成分及心肌細胞保護作用。綜合運用硅膠、Sephadex LH-20、MCI、半制備液相等多種色譜分離方法,對小葉黃楊中等極性部位進行分離純化,采用波譜學技術對分離的單體化合物進行結構鑒定。另外,對提取各部位和分離得到的16個化合物進行體外心肌細胞保護作用測試。從小葉黃楊干燥葉中共分離得到14個化合物,分別為香草酸乙酯(1、香草醛(2、花椒毒素(3、反式對羥基肉桂酸乙酯4)、3,4,5-trimethoxycinnamyl alcohol5、丁香酸乙酯(6、(S)-5-hydroxy-3,4-dimethyl-5-pentylfuran-2(5H)-one 7、樺木酸(8、4-羥基-3,5-二甲氧基苯甲醛9、7,3′,4′-三甲基槲皮素(10、白樺脂醇(11、penduletin12、23-O-(E)-p-coumaroyl-23-hydroxybetulin13、松脂素(14。其中化合物2、56為首次從該植物中分離得到,體外實驗表明EA部位和化合物14(松脂素)可顯著改善H2O2誘導的心肌細胞損傷。

    關鍵詞:小葉黃楊;化學成分;心肌保護作用;H9c2細胞

    中圖分類號:O629.9      文獻標識碼:A       文章編號:0258-32832022--

     

    Chemical constituents and cardioprotective effects of Buxus Sinica var. parvifolia M. Cheng

    WANG Rui1, ZHANG Yan1, MUHAMMAD Ishaq1, TIAN Yan2, FU Deng-lin2, YU Hua-jun*2, XIAO Xue3, YAN Shi-kai1,2,3, JIN Hui-zi*1 (1. School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China; 2. Guizhou Jingcheng Pharmaceutical Co., Ltd, Guiyang 550200, China; 3. Institute of Chinese Medicinal Sciences, Guangdong Pharmaceutical University, Guangzhou 510006, China), Huaxue Shiji, 2022, 44(8),

    Abstract: The chemical constituents from the leaves of Buxus Sinica var. parvifolia M. Cheng and their cardioprotective bioactivities were studied. The chemical constituents from the ethyl acetate (EA) part of this plant were isolated and purified by column chromatography such as silica gel, Sephadex LH-20, MCI, and preparative HPLC. The structures of isolates were elucidated by spectroscopic analyses. A hydrogen peroxide (H2O2)-induced cardiomyocyte line H9c2 was used as an in vitro model of damaged cardiomyocytes to evaluate the effects of the extracts and the isolates. Fourteen compounds were isolated and elucidated as ethyl 4-hydroxy-3-methoxybenzoate (1), vanillin (2), xanthotoxin (3), trans-p-hydroxycinnamic acid ethyl ester (4), 3,4,5-trimethoxycinnamyl alcohol (5), syringic acid ethyl ester (6), (S)-5-hydroxy-3,4-dimethyl-5-pentylfuran-2(5H)-one (7), betulinic (8), 4-hydroxy-3,5-dimethoxybenzaldehyde (9), 7,3′,4′-trimethylquercetin (10), betulin (11), Pendleton (12), 23-O-(E)-p-coumaroyl-23-hydroxybetulin (13) and pinoresinol (14). Compounds 2, 5, and 6 were firstly isolated from this plant. The EA part and compound 14 (pinoresinol) showed significant protective effects against H2O2-induced cardiomyocyte injury in H9c2 cells.

    Key words: Buxus sinica; chemical constituents; cardioprotective effects; H9c2 cells

    引用本文:王瑞,張巖,MUHAMMAD Ishaq,等. 小葉黃楊化學成分及心肌細胞保護作用研究[J]. 化學試劑,2022,44(8): 1111-1117。

     

     

    突變異檸檬酸脫氫酶抑制劑治療膠質瘤的研究進展

    王健博1,2a,孟曉燕2a,張雍鑫2a,孔曉華2a,徐中琦2a,李興偉2a,靳京2a,楊天明*2a,2b,黃長江*2a,2b

    1. 內蒙古醫科大學 藥學院,內蒙古 呼和浩特 010110;2. 天津藥物研究院a. 天津市新藥設計與發現重點實驗室,b. 釋藥技術與藥代動力學國家重點實驗室,天津 300301

     

    摘要:膠質瘤常伴隨異檸檬酸脫氫酶的突變,催化α-酮戊二酸轉變為2-羥基戊二酸并大量蓄積,導致DNA/RNA甲基化,影響細胞分化。突變異檸檬酸脫氫酶抑制劑通過與腫瘤細胞中突變體特異性結合,使其失去催化α-酮戊二酸為2-羥基戊二酸的功能,引起下游信號通路的改變,達到抑制腫瘤生長的效果??偨Y突變異檸檬酸脫氫酶抑制劑治療膠質瘤的研究進展,重點介紹作用機制、共晶結構、臨床試驗等,并且討論了發展方向。

    關鍵詞:膠質瘤;突變異檸檬酸脫氫酶;抑制劑;2-羥基戊二酸;共晶結構

    中圖分類號:R979.1      文獻標識碼:A      文章編號0258-32832022--

     

    Progress of Inhibitors of MutantIsocitrate Dehydrogenase for the Treatment of Gliomas WANG Jian-bo1,2a, MENG Xiao-yan2a, ZHANG Yong-xin2a, KONG Xiao-hua2a, XU Zhong-qi 2a, LI Xing-wei2a, JIN Jing 2a, YANG Tian-ming *2a,2b, HUANG Chang-jiang*2a,2b(1. School of Pharmacy, Inner Mongolia Medical University, Hohhot 010110, China; 2a. Tianjin Key Laboratory of Molecular Design and Drug Discovery, 2b. State Key Laboratory of Drug Delivery Technology and Pharmacokinetics, Tianjin Institute of Pharmaceutical Research, Tianjin 300301, China), Huaxue Shiji,2022,44 (8), ~

    AbstractGlioma is often accompanied by mutations in isocitrate dehydrogenase, which convert α-ketoglutarate (α-KG) into 2-hydroxyglutarate (2-HG), resulting in the accumulation of 2-HG, subsequently leading to DNA/RNA methylation that affects cell differentiation. The mutant isocitrate dehydrogenase inhibitors specifically bind to the mutant enzyme in tumor cells, causing the loss of the activity of catalyzing α-KG to 2-HG, and resulting in the changes of downstream signaling pathways to achieve the inhibition of tumor growth. This article summarizes the research progress of mutant isocitrate dehydrogenase inhibitors for the treatment of gliomas, emphasizing mechanism, cocrystal structures, and clinical trials, and discusses the development direction of this field.

    Keywords: gliomas; mutant isocitratedehydrogenase; inhibitors; 2- hydroxyglutarate; cocrystal structures

    引用本文:王健博,孟曉燕,張雍鑫,等. 突變異檸檬酸脫氫酶抑制劑治療膠質瘤的研究進展 [J]. 化學試劑, 2022, 44(8): 1118-1127。

     

     

    雷公藤甲素丁二酸單酯對A549/DDP細胞的抑制作用研究

    楊俊1,王丹丹2,梁玉清1,丁麗娜1,卓俊睿1,梁光平*1

    1. 遵義醫藥高等??茖W校,貴州 遵義  563006;2. 銅仁職業技術學院,貴州 銅仁 554300

    摘要研究雷公藤甲素丁二酸單酯(YJ-4)對A549/DDP抑制作用及其機制。以雷公藤甲素為原料,與丁二酸酐在DMAP/Pyridine催化下反應后得到化合物YJ-4,其結構經1HNMR,13CNMRHR-ESI-MS表征,采用MTT法評價其對人非小細胞肺癌細胞(A549)、人肺腺癌耐順鉑株(A549/DDP)、人乳腺癌細胞(MCF-7)的體外抗腫瘤活性;不同濃度的化合物YJ-4作用于A549/DDP細胞后,DAPI染色法檢測細胞核狀態,PI染色法檢測細胞周期,Annexin V-FITC/PI雙染法檢測細胞凋亡;分子對接軟件Autodock來評價化合物YJ-4MDM2蛋白結合的能力?;衔?/span>YJ-4A549/DDP33.32 ± 3.55 μmol/L)、A5494.31 ± 1.01 μmol/L)、MCF-716.08 ± 2.63 μmol/L細胞株均具有良好的細胞毒性,是陽性對照藥順鉑的數倍,且通過阻A549/DDP細胞周期G2/M期,從而誘導細胞凋亡,與MDM2GLY-16氨基酸殘基與形成氫鍵(d=1.9 ?),結合能(affinity)為 -8.4 kcal/mol,能夠較好的結合?;衔?/span>YJ-4對耐藥細胞株A549/DDP細胞具有良好的細胞毒活性,其作用機制為促進A549/DDP細胞凋亡、阻滯細胞周期G2/M期,可能與抑制MDM2蛋白和p53相互作用有關。

    關鍵詞  雷公藤甲素丁二酸單酯;衍生物;人肺癌耐順鉑株A549/DDP;體外抗腫瘤活性

    中圖分類號:R914.4    文獻標識碼:A    文章編號:0258-32832022--

     

    Antitumor Activities of Triptolide Succinate on A549/DDP Lung Cancer YANG Jun1, WANG Dan-dan2, LIANG Yu-qing1, DING Li-na1, ZHUO Jun-rui1, LIANG Guang-ping*11. Zunyi Medical And Pharmaceutical College, Zunyi 563006, China; 2. Tongren Polytechnic College, Tongren 554300, China), Huaxue Shiji,2022,44 (8),00 ~ 00

    Abstract: To investigate the effects and mechanisms of triptolide succinate monoester (YJ-4) on cisplatin-resistant human lung adenocarcinoma cells (A549/DDP). Compound YJ-4 was synthesized by catalyzing triptolide and succinic anhydride under DMAP/pyridine. Its structure was characterized by 1HNMR, 13CNMR, and HR-ESI-MS. Its anti-tumor activity in vitro against human non-small cell lung cancer cells (A549), human breast cancer cells (MCF-7), and A549/DDP cells were evaluated using the MTT method. After A549/DDP cells were treated with YJ-4 at different concentrations, the nuclear state was detected by DAPI staining, the cell cycle was detected by PI staining, and the apoptosis was detected by Annexin V-FITC/PI double staining. The binding ability of YJ-4 to MDM2 protein was evaluated using molecular docking software Autodock. Compound YJ-4 presented high cytotoxicity to A549/DDP33.32 ± 3.55 μmol/L, A5494.31 ± 1.01 μmol/L, and MCF-716.08 ± 2.63 μmol/Lcells, which was significantly superior to the positive control drug cisplatin. Additionally, YJ-4 blocked the G2/M phase of the A549/DDP cell cycle and induced apoptosis. It could form a hydrogen bond with amino acid residue GLY-16 of MDM2 (d=1.9 ?), with an affinity of -8.4 kcal/mol, suggesting a high binding ability. Compound YJ-4 has a high cytotoxic activity to drug-resistant cell line A549/DDP. Its mechanism is to promote A549/DDP cell apoptosis and block the G2/M phase of the cell cycle, which may be related to the inhibition of the interaction between MDM2 protein and p53.Key words: C14-triptolide succinate monoester; derivatives; Cisplatin-resistant human lung cancer cells; antitumor activity in vitro

    引用本文楊俊, 王丹丹, 梁玉清, . 雷公藤甲素丁二酸單酯對A549/DDP細胞的抑制作用研究[J]. 化學試劑, 2022, 44(8): 1128-1135。

     

     

    喹啉類mTOR/HDAC雙靶抑制劑的設計、合成與體外活性評價

     

    李志,張明明,陶強強,何格,趙燦,鐘國琛*,馬曉東*

    (安徽中醫藥大學 藥學院 安徽省中醫藥科學院藥物化學研究所,安徽 合肥  230012

     

    摘要:為發現新型mTOR/HDAC雙靶抑制劑,基于藥效團融合策略構建目標分子,并經親核取代或縮合反應、羥胺解反應制得目標分子。體外抑酶活性測試結果顯示,4'-((4-(4-(N-羥基戊酰胺)-哌嗪-1-)-3-(三氟甲基)苯基)氨基)-[3,6'-二喹啉]-3'-甲酰胺呈現出中等強度的雙靶抑酶活性(Mtor、HDAC1、HDAC6IC50 值分別為1444、832、230 nmol/L);4'-((4-(4-(N-羥基乙酰胺)-哌嗪-1-)-3-(三氟甲基)苯基)氨基)-[3,6'-二喹啉]-3'-甲酰胺mTOR具有良好的抑制活性IC50 = 64 nmol/L)??乖鲋郴钚詼y試結果顯示,所有目標分子A549細胞株的增殖抑制活性與陽性對照SAHA、MLN-0128相當或略優;4'-((4-(4-(N-羥基-1-羰基辛酰)哌嗪-1-)-3-(三氟甲基)苯基)氨基)-[3,6'-二喹啉]-3'-甲酰胺HCT116的抗增殖活性與MLN-0128相當。

    關鍵詞mTOR;HDAC;雙靶抑制劑;抑酶活性;抗增殖活性

     

    Quinoline Derivatives of mTOR/HDAC Dual-Target Inhibitors : The Design, Synthesis and In vitro Biological Evaluation LI Zhi, ZHANG Ming-ming, TAO Qiang-qiang, HE Ge, ZHAO Can, ZHONG Guo-chen*, Ma Xia-odong* (School of Pharmacy, Anhui University of Chinese Medicine, Department of Medicinal Chemistry, Anhui Academy of Chinese Medicine, Hefei, Anhui 230031, China), Huaxue Shiji, 2022, 44(8),

    AbstractTo discover novel mTOR/HDAC bi-functional inhibitors, target compounds were designed via a pharmacophore-merging strategy and prepared by nucleophilic substitution or condensation and the following hydroxylaminolysis. As demonstrated by the in vitro enzymatic assay, compound 14 exhibited moderate inhibitory activity against both mTOR and HDAC (mTOR IC50 = 1444 nmol/L; HDAC1 IC50 = 832 nmol/L; HDAC6 IC50 = 230 nmol/L). Besides, compound 13 displayed acceptable inhibitory activity against mTOR (IC50 = 64 nmol/L). In the anti-proliferative assay, all the synthesized compounds exhibited comparable or superior activity to the positive control SAHA and MLN-0128 against the A549 cell line. Additionally, compound 16 exerted comparable anti-proliferative activity to MLN-0128 against the HCT116 cell line.

    Key wordsmTOR; HDAC; bi-functional inhibitors; inhibitory activity against both mTOR and HDAC; anti-proliferative activity

    引用本文:李志, 張明明, 陶強強, . 喹啉類mTOR/HDAC雙靶抑制劑的設計、合成與體外活性評價[J]. 化學試劑, 2022, 4481136-1141.

     

     

    基于甘草酸的熒光納米碳點的合成及性能研究

    黃湘,周莉佳,粟小燕,裴叔宸,柴水琴,管天冰*

    (重慶科技學院 化學化工學院,重慶 401331) 

    摘要隨著抗生素在臨床上濫用,開發新型的抗菌納米材料顯得尤為重要。本研究以甘草酸為原料,經一步水熱法合成了的新型熒光納米碳點材料并進行結構表征。碳點粒徑分布范圍為3.05.3 nm,厚度為3.04.0 nm,表面富含羧基、羥基、碳碳雙鍵等官能團。熒光光譜中,碳點的最大激發波長為360 nm,最大發射波長為430 nm。碳點對微生物具有抑制作用,其中對金黃色葡萄球菌的MIC值為0.60 mg/mL,對大腸桿菌的MIC值為0.60 mg/mL。實驗結果表明,該碳點具有穩定的熒光特性和良好的抗菌活性,有望在多功能生物醫學納米材料領域得到更廣泛的應用。

    關鍵詞甘草酸; 碳點; 納米材料; 熒光性質; 抗菌活性       

    中圖分類號:O613.71    文獻標識碼:A       文章編號:,0258-32832022--

     

    Synthesis, Fluorescence Properties and Antibacterial Activity of Fluorescent Carbon Dots Based on Glycyrrhizic Acid   HUANG Xiang, ZHOU Li-jia, SU Xiao-yan, PEI Shu-chen, CHAI Shui-qin, GUAN Tian-bing (College of Chemistry and Chemical Engineering, Chongqing University of Science and Technology, Chongqing 401331, China), Huaxue Shiji, 2022, 44(8),

    AbstractWith the abuse of antibiotics clinically, the development of new antibacterial nanomaterials is particularly important. In this study, a new type of fluorescent carbon dot was synthesized by a one-step hydrothermal method with glycyrrhizic acid and citric acid as raw materials, and the structure was characterized. The results show that the carbon dots have a particle size distribution range of 3.0  5.3 nm and a thickness of 3.0-4.0 nm. The surface is rich in functional groups such as carboxyl groups, hydroxyl groups, and carbon-carbon double bonds. In the fluorescence spectrum, the maximum excitation wavelength of carbon dots is 360 nm, and the maximum emission wavelength is 430 nm. Through the Minimum Inhibitory Concentration (MIC) experiment, it is determined that the carbon dot has an inhibitory effect on various microorganisms. Among them, the MIC value for Staphylococcus aureus is 0.60 mg/mL, and for Escherichia coli is 0.60 mg/mL. Experimental results show that the carbon dots have stable fluorescence characteristics and good antibacterial activity, and are expected to be more widely used in the field of multifunctional biomedical nanomaterials.

    Key wordsglycyrrhizic acid; carbon dots; nano materials; fluorescent property; antibacterial activity

    引用本文黃湘,周莉佳,粟小燕,等. 基于甘草酸的熒光納米碳點的合成及性能研究[J]. 化學試劑, 2022, 44(8): 1142-1147.

     

     

    β-FeOOH改性凹凸棒土的制備及其對單寧酸吸附性能研究

    袁大英1,張紅軍1,潘緒華1,徐軼群2,胡慶松*2

    1. 中交上海航道局有限公司 江蘇交通建設工程分公司,江蘇 南京  210000;2. 揚州大學 環境科學與工程學院,江蘇 揚州  225000

    摘要:為了提高凹凸棒土對單寧酸的吸附性能,采用水浴法制備β-FeOOH改性凹凸棒土(ATP/β-FeOOH)吸附劑。通過X射線衍射儀、X射線光電子能譜儀和紅外光譜儀分析吸附劑的組成和化學基團,通過透射電子顯微鏡和比表面積分析技術觀察吸附劑的形貌和孔徑分布。以單寧酸為目標污染物,進行吸附動力學和吸附等溫線實驗,考察了吸附劑用量、污染物濃度、初始pH值和共存離子對吸附劑去除單寧酸效能的影響。吸附實驗結果表明:ATP/β-FeOOH吸附單寧酸過程符合擬二級動力學模型,Langmuir模型比Freundlich模型更能反映吸附過程。其中,30 wt% ATP/β-FeOOH的吸附性能最佳,最高吸附容量可以達到38.63 mg/g,并確定最佳吸附條件為溶液初始pH3.0,吸附劑投加量為1.0 g/L。本研究結果表明:β-FeOOH的引入顯著增強了凹凸棒土對單寧酸的吸附性能,此外,ATP/β-FeOOH對單寧酸的吸附機理可以歸結為螯合作用和靜電作用。

    關鍵詞:丹寧酸;凹凸棒土;改性;羥基氧化鐵;吸附

    中圖分類號:X5     文獻標識碼:A      文章編號:0258-32832022--

     

    Construction of β-FeOOH modified Attapulgite adsorbent and its Adsorption Property for the removal of Tannin YUAN Da-ying1, ZHANG Hong-jun1, PAN Xu-hua1, XU Yi-qun2, HU Qing-song*2 (1. Shanghai Dredging CO., LTD. Jiangsu Traffic Construction Engineering Branch, Nanjing 210000, China; 2. College of Environmental Science and Engineering, Yangzhou University, Yangzhou 225000, China), Huaxue Shiji,2022,44 (8),00 ~ 00

    Abstract: As a kind of water-soluble polyphenol, tannin is widely employed in coating, food additives, and deodorants. It can pose a severe threat to human health after entering into aqueous environments. Among various technologies for eliminating tannin, adsorption is deemed a promising technology. Nevertheless, traditional adsorbents, like activated carbon, and attapulgite, are limited in their adsorption capacity. In order to improve the adsorption capacity of tannin over attapulgite, β-FeOOH modified attapulgite adsorbent is prepared via hydrothermal method. X-ray diffractometer, X-ray photoelectron spectrometer, and infrared spectrometer are employed to analyze the composition and chemical bond of the obtained samples. And the morphology and pore diameter distributes are acquired on account of transmission electron microscope and specific surface area analysis techniques. Tannin is selected as the target pollutant, and the adsorption kinetics and isotherm experiments are carried out. The effects of the amount of adsorbent, pollutant concentration, initial pH value, and coexisting ions on the removal efficiency of tannin are investigated. The experimental results demonstrate that the adsorption process abides by the pseudo-second-order model. And Langmuir model can simulate the adsorption process better than Freundlich model. Among these, 30 wt% ATP/β-FeOOH displays the best adsorption performance. And the highest adsorption capacity can reach 38.63 mg/g. The optimal adsorption conditions are initial pH value (3.0) and an adsorbent of dosage 1.0 g/L. This work indicates that the introduction of β-Obviously improves the adsorption performance of tannin. And the adsorption mechanism can be attributed to chelation and electrostatic interaction.

    Key words: tannin; attapulgite; modification; FeOOH; adsorption

    引用本文:袁大英,張紅軍,潘緒華,等. β-FeOOH改性凹凸棒土的制備及其對單寧酸吸附性能研究[J]. 化學試劑, 2022, 44(8): 1148-1156。

     

     

    液晶型適配體生物傳感器無標記快速檢測黏蛋白1

    潘興隆1,于依楠1,李寧偉1,武雅靜2,侯利杰1,申炳俊1,金麗虹*1

    (1. 長春理工大學 生命科學技術學院,吉林 長春  130022;2. 長春理工大學 文學院,吉林 長春  130022)

     

    摘要:構建了一種基于適配體分子識別的液晶型生物傳感器,用于人體血液腫瘤標志物黏蛋白1MUC1無標記快速檢測。傳感器由下玻片、銅載網和上玻片組成,下玻片通過表面活性劑、硅烷化試劑修飾及固定適配體,誘導4-氰基-4'-戊基聯苯5CB向列型液晶分子的垂直排列取向。傳感器中適配體與MUC1特異性結合可破壞5CB原有垂直排列取向,導致其偏光顯微圖像由,根據圖像亮區覆蓋率Br變化可實現MUC1定量檢測。結果表明,文中編寫的MATLAB程序可實現偏光顯微圖像Br自動計算;1 fg/mL  1 μg/mL范圍內,MUC1濃度對數與Br間存在線性關系Br = 7.979 9 LogCMUC1 +11.824 65,R2 = 0.984 39,MUC1檢測限LOD達到0.47 fg/mL。液晶型適配體生物傳感器具有較高的檢測靈敏度及特異性,實現了人體血液樣本MUC1有效檢測,其有望應用于臨床MUC1檢測。

    關鍵詞:黏蛋白1;偏振光顯微技術;適配體;液晶;生物傳感器

    中圖分類號:TP212.3      文獻標識碼:A      文章編號:0258-32832022--

     

    A Liquid Crystal-based Aptasensor for Rapid Detection of MUC1 without Labeling PAN Xing-long1, YU Yi-nan1, LI Ning-wei1, Wu Ya-jing2, Hou Li-jie1, SHEN Bing-jun1, JIN Li-hong*1. (1. School of Life Science and Technology, Changchun University of Science and Technology, Changchun 130022, China; 2. School of Liberal Arts, Changchun University of Science and Technology, Changchun 130022, China) , Huaxue Shiji,2022,44 (8),00 ~ 00

    Abstract: A liquid crystal biosensor based on aptamer molecular recognition was constructed for rapid detection of human blood tumor marker mucin1(MUC1) without labeling. The sensor was composed of a lower slide, a copper substrate, and an upper slide. The lower slide was modified and immobilized by surfactant and silanization reagent to induce the homeotropic orientation of the nematic liquid crystal molecules of 4-cyano-4’-amyl biphenyl (5CB). The specific binding of MUC1 with the aptamer in the sensor can destroy the original vertical alignment of 5CB, resulting in the polarized optical microscopic image changing from dark to bright. Quantitative detection of MUC1 can be achieved according to the change of bright coverage (Br) in the image. The results show that the MATLAB program programmed in this paper can realize the automatic calculation of Br in the polarized optical microscopy image. The concentration of MUC1 is in the range of 1 fg/mL~1 μg/mL, and there is a linear relationship between its logarithmic concentration and Br (Br = 7.9799 LogCMUC1 + 11.82465, R2 = 0.98439). The detection limit (LOD) of MUC1 was 0.47 fg/mL. The liquid crystal biosensor based on aptamer has high detection sensitivity and specificity, realizing the effective detection of MUC1 in human blood samples, and it is expected to be applied in clinical MUC1 detection.

    Keywords: MUC1; polarized optical microscopy; aptamer; liquid crystal; biosensor

    引用本文潘興隆,于依楠,李寧偉,等. 液晶型適配體生物傳感器無標記快速檢測黏蛋白1[J]. 化學試劑, 2022, 44(8): 1157-1163。

     

     

    兩例基于對氯苯乙酸配體構筑的銅(II)配合物晶體結構及熒光性能測試

     

    李波1,沈紅*1,王霏宇1,毛逢銀2,李勇輝1

    1. 宜賓職業技術學院,四川 宜賓  644000;2. 四川輕化工大學        ,四川 自貢  643000

     

    摘要:室溫下,通過溶劑揮發法合成了對氯苯乙酸鄰菲啰啉銅(II)配合物(C28H20Cl2CuN2O4)和對氯苯乙酸2,2'-聯吡啶銅(II)配合物(C26H22Cl2CuN2O5)。用X射線單晶衍射測定了配合物的晶體結構;結果顯示,配合物C28H20Cl2CuN2O4屬于三斜晶系,P1(——)空間群,每個不對稱單元由一個銅(II)離子,兩個對氯苯乙酸配體及一個鄰菲啰啉配體組成。配合物C26H22Cl2CuN2O5屬于單斜晶系,P21/n空間群;每個不對稱單元由一個銅(II)離子,兩個對氯苯乙酸配體及一個2,2'-聯吡啶配體組成。在熒光光譜上,配合物C28H20Cl2CuN2O4的最強激發峰和發射峰在分別在380 nm430 nm,配合物C26H22Cl2CuN2O5的最強激發峰和發射峰分別在380 nm430 nm;兩個配合物在室溫下穩定。

    關鍵詞:銅(II)配合物;對氯苯乙酸;晶體結構;1,10-鄰菲啰啉;2,2'-聯吡啶

    中圖分類號:O614.121          文獻標識碼:A        文章編號:0258-32832022--

     

    Crystal Structure and Fluorescence Performance Testing of Two Copper (II) Complexes Based on 4-Chlorophenylacetic Acid Ligands Li Bo1, Shen Hong*1, Wang Fei-yu1, Mao Feng-yin2, Li Yong-hui1 (1. Yibin Vocational Technical College, Yibin Sichuan 644000; 2 Sichuan University of Science & Engineering, Zigong Sichuan 643000, China), Huaxue Shiji, 2022, 448,~

    AbstractThe copper(II) complex [C28H20Cl2CuN2O4] (4-chlorophenylacetic acid, 1,10-phenanthroline) and complex [C26H22Cl2CuN2O5] (4-chlorophenylacetic acid, 2,2'-bipyridine) were synthesized via solvent evaporation method. Their crystal structures were determined by the crystal X-ray diffraction method. The results show that complex [C28H20Cl2CuN2O4] crystallizes in the triclinic space group P1(——) with each asymmetric unit consisting of one Cu(II) ions, two 4-chlorophenylacetic acid ligands, and one 1,10-phenanthroline ligand. Complex [C26H22Cl2CuN2O5] crystallizes in the monoclinic with space group P21/n with each asymmetric unit consisting of one Cu(II) ions, two 4-chlorophenylacetic acid ligand, s and one 2,2'-bipyridine ligands. The excitation peak of complex [C28H20Cl2CuN2O4] was 380 nm. The emission peak was 430 nm, the excitation peak of complex C26H22Cl2CuN2O5 was 380 nm, the and emission peak was 430 nm. Two complexes are stable at room temperature.

    Key wordscopper(II) complex; 4-chlorophenylacetic acid; crystal structure; 1,10-phenanthroline; 2,2'-bipyridine

    引用本文:李波, 沈紅, 王霏宇, . 兩例基于對氯苯乙酸配體構筑的銅(II)配合物晶體結構及熒光性能測試[J]. 化學試劑, 2022, 4481164-1169.

     

     

    超聲酶法輔助提取水芹菜多糖工藝優化及生物學活性研究

    張臘梅,黃紅琴,李敏,茍鼎

    (達州中醫藥職業學院,四川 達州  635000

     

    摘要:采用超聲酶法輔助提取水芹菜多糖并研究其生物活性。采用單因素及響應面法優化研究超聲酶法輔助提取水芹菜多糖提取工藝,并通過水芹菜多糖清除?OH自由基、DPPH自由基、ABTS+自由基及鐵還原力來分析其抗氧化能力和測定DNA超螺旋結構含量評價DNA氧化損傷保護。水芹菜多糖的最佳提取條件為:料液比1:30 (g:mL)、超聲時間40 min、超聲功率400 W、提取溫度50 ℃、纖維素酶添加量3.6%,水芹菜多糖得率為18.92 %。水芹菜多糖有較強的清除?OH自由基、DPPH自由基、ABTS+自由基能力及鐵還原力。水芹菜多糖對抑制DNA損傷具有顯著作用。0.04 mg/mL時有最強的保護率,為63.23%。水芹菜多糖具有很強的生物學活性,可以作為一種天然食品添加劑。

    關鍵詞:水芹菜;多糖;超聲酶法提??;抗氧化;DNA氧化損傷

    中圖分類號:R284      文獻標識碼: A        文章編號:0258-32832022--

     

    Optimization of Extraction Technology of Polysaccharide from Oenanthe Javanica by Ultrasonic and Enzyme-assisted Extraction and Its Biological Activities ZHANG La-mei1, HUANG Hong-qin, LI Min, GOU Ding ( Dazhou Vocational College of Chinese Medcine, Dazhou 635000, China ) , Huaxue Shiji,2022,44 (8),00 ~ 00

    Abstract To extract polysaccharides from Oenanthe javanica by ultrasonic and enzyme-assisted, biological activity was studied. The ultrasonic and enzyme-assisted extraction process of polysaccharides from Oenanthe javanica was optimized by single factor and response surface methodology. The antioxidant activity was evaluated by the ability to scavenge ?OH radical, DPPH, ABTS+, and iron reduction, and the protection against DNA oxidative damage was evaluated by measuring the content of DNA super helixix structure. The optimum extraction conditions were as follows: material-to-water ratio 1:30 (g: mL), ultrasonic time 50 min, ultrasonic power 400 W, extraction temperature 65 , cellulose amount 3.6%, and the yield of polysaccharide from Oenanthe javanica was 18.92%. Polysaccharides from Oenanthe javanica had a strong ability to scavenge ·OH radical, DPPH radical, ABTS+ Radical and iron reduction. Polysaccharides from Oenanthe javanica had a significant effect on protecting activity against DNA damage, and the strongest protective rate was 0.04 mg/mL, which was 63.23Polysaccharideside from Oenanthe javanica had strong biological activity and could be used as a natural food additive.

    Key words: Oenanthe javanica; polysaccharide; ultrasonic and enzyme-assisted extraction; antioxidation; oxidative DNA damage

    引用本文:張臘梅,黃紅琴,李敏,等. 超聲酶法輔助提取水芹菜多糖工藝優化及生物學活性研究 [J]. 化學試劑, 2022, 44(8): 1170-1177。

     

     

    超聲-微波協同輔助提取藍莓花色苷及其抗腫瘤活性研究

    姚會敏1,孟宇竹2,李向果1,耿曉東*1,3

     

    1. 河南質量工程職業學院 食品與化工學院,河南 平頂山 467000;2. 平頂山技師學院 現代服務系,河南 平頂山 467000;3. 河南農業大學 林學院,河南 鄭州 450002

     

    摘要:本文以藍莓為原料,探究超聲-微波協同輔助提取Ultrasonic-microwave assisted extraction,UMAE藍莓花色苷工藝及其抗腫瘤活性。在單因素實驗的基礎上,通過正交實驗優化UMAE藍莓花色苷的工藝,同時利用掃描電鏡觀察藍莓顆粒微觀結構。通過MTT法研究在最優提取工藝下獲得的藍莓花色苷提取物(Blueberry anthocyanins extracts,BAEs)對A549細胞存活率的影響。采用全光譜流式細胞儀測定BAEsA549細胞凋亡的影響。結果表明UMAE藍莓花色苷最優工藝參數為超聲功率500 W、微波功率100 W和乙醇體積分數60%,在此條件下,藍莓花色苷得率為(7.15±0.13 mg/g。通過掃描電鏡觀察經超聲-微波、超聲和微波處理后藍莓細胞微觀結構,對比發現超聲-微波處理后藍莓細胞壁發生不同程度破裂,說明UMAE具有強化提取花色苷的作用。BAEs在質量濃度為1080 mg/mL范圍內,BAEs濃度增加A549細胞存活率顯著降低,而凋亡率顯著增加。研究結果為藍莓深加工提供重要依據。

    關鍵詞:超聲-微波協同輔助提??;藍莓;花色苷;工藝;抗腫瘤活性

    中圖分類號:R284.2      文獻標識碼:A      文章編號:0258-32832022--

     

    Ultrasonic-microwave Assisted Extraction of Anthocyanins from Blueberry and Its Antitumor Activity YAO Hui-min1, MENG Yu-zhu2, LI Xiang-guo1, GENG Xiao-dong*1,31. Food and Chemical Engineering Department, Henan Quality Polytechnic, Pingdingshan 467000, China; 2. Modern Service Department, Pingdingshan Institute Technology, Pingdingshan 467000, China; 3. College of Forestry, Henan Agricultural University, Zhengzhou 450002,China,Huaxue Shiji, 2022, 44(8),

    Abstract: In this paper, blueberry was used as raw material to explore the ultrasonic-microwave-assisted extraction process of blueberry anthocyanins and its antitumor activity. The process of UMAE anthocyanins from blueberry anthocyanins was optimized by an orthogonal experiment based on a single factor experiment, and the microstructure of blueberry particles was observed by a scanning electron microscope. The effect of blueberry anthocyanins extracts (BAEs) obtained under the optimal extraction parameters on the survival rate of A549 cells was measured by the MTT method. The effect of BAEs on apoptosis of A549 cells was determined by full-spectrum flow cytometry. The results showed that the optimum extraction parameters to achieve the highest anthocyanins yield (7.15±0.13) mg/g from blueberry by UMAE were obtained under the ultrasonic power of 500 W and the microwave power of 1 W, and ethanol concentration of 60%. The microstructure of blueberry cells treated with ultrasound-microwave, ultrasound, and microwave was observed by scanning electron microscope. It was found that the cell wall of blueberry was broken in varying degrees after ultrasound-microwave treatment, indicating that UMAE can strengthen the extraction of anthocyanins. In the mass concentration range of 1080 mg/mL, the survival rate of A549 cells decreased significantly and the apoptosis rate increased obviously with the increase in BAEs concentration. The findings provide an important basis for the further processing of blueberries.

    Keywords: ultrasonic-microwave assisted extraction; blueberry; anthocyanins; process; antitumor activity

    引用本文:姚會敏,孟宇竹,李向果,等. 超聲-微波協同輔助提取藍莓花色苷及其抗腫瘤活性研究[J]. 化學試劑,2022,44(8): 1178-1183。

     

     

    基于二苯并噻吩砜多孔聚合物光解水制氫研究

     

    王首明,黃曉鋒,羅錦新,金耀城*,霍延平*

    (廣東工業大學 輕工化工學院,廣東 廣州  510006

     

    摘要制備了兩種基于二苯并噻吩砜單元的新型有機共軛多孔聚合物PBDFSOPBDTSO,并將其應用于光水制氫領域,通過主鏈含氧/硫雜原子修飾取代,系統研究了主鏈結構對材料光學吸收、化學能級及光催化性能的影響。研究發現,兩種共軛多孔聚合物都具有較寬的光吸收范圍,合適的光學帶隙,并具有光解水制氫的能力。其中,含硫原子多孔聚合物PBDTSO在使用抗壞血酸作為犧牲劑時,模擬太陽光照射下展現出1973 μmol/(g·h)的析氫速率,高于含氧原子的多孔聚合物PBDFSO的析氫速率,并具有較好的光穩定性。這表明通過雜原子取代可以優化多孔聚合物結構,從而有效提高聚合物催化劑的光催化活性。

    關鍵詞共軛多孔聚合物;二苯并噻吩砜;苯并雙噻吩;苯并雙呋喃;光催化水制氫

    中圖分類號:O631.1+1     文獻標識碼:A       文章編號:0258-32832022--

     

    Photocatalytic Performance of Organic Porous Polymers Based on Dibenzothiophene Sulfone Unit WANG Shou-ming, HUANG Xiao-feng, LUO Jin-xin, JIN Yao-cheng*, HUO Yan-ping* (School of Chemical Engineering and Light Industry, Guangdong University of Technology, Guangzhou 510006, China), Huaxue Shiji, 2022, 44(8),~

    AbstractIn recent years, significant progresses have achieved in the design and preparation of conjugated organic polymer photocatalysts. However, developing organic polymer photocatalysts with high conversion efficiency is still challenging. The rational structural design of organic polymer photocatalysts is the key to achieving high photocatalytic performance. Here, two novel organic conjugated porous polymers PBDFSO and PBDTSO based on a dibenzothiophene sulfone unit were prepared and applied to photocatalytic hydrogen production from water. The chemical structures and their influence on the absorption spectrum, energy level, and photocatalytic performance of the materials was systematically studied. The two prepared porous polymers had a wide optical absorption range and suitable optical band gap, and both two polymers could produce hydrogen by photocatalytic water. The results show that the sulfur atom-containing porous polymer PBDTSO exhibits a hydrogen evolution rate of 1973 μmol?g-1h-1 when ascorbic acid is used as a sacrificial agent under simulated sunlight irradiation, which is higher than that of the oxygen atom-containing porous polymer PBDFSO and has good photostability. It indicates that the porous polymer structure can be optimized by heteroatom substitution, which can effectively improve photocatalytic activity.

    Key wordsconjugated porous polymers; dibenzothiophene sulfone; benzodisthiophene; benzodisfuran; photocatalytic hydrogen production from water

    引用本文:王首明, 黃曉鋒, 羅錦新, . 基于二苯并噻吩砜多孔聚合物光解水制氫研究[J]. 化學試劑, 2022, 4481184-1190.

     

     

    在線監測直接進樣和罐采樣方法一次性分析117組分VOCs的比較

     

    王瀟,王成然,李志昂,王凱,周鑫*

    (中國測試技術研究院,四川 成都  610021

     

    摘要:使用蘇瑪罐采樣與模擬在線監測直接進樣兩種方法,通過預濃縮-氣相色譜-火焰離子化檢測-質譜檢測器GC-FID-MS)系統對稀釋至5 nmol/mol濃度的117組分VOCs標準氣體進行分析。以直接進樣的結果為標準,分析罐采樣方法,結果發現蘇瑪罐對甲醛和丁烯醛較明顯的吸附,甲醛降低32%,丁烯醛降低12%,其余組分的相對偏差10%以內,RSD0.5% ~ 8%。之后在加濕(60%RH)與不加濕條件下比較117VOCs在蘇瑪罐中的響應,結果發現甲醛含量在加濕條件下繼續降低18%。蘇瑪罐采樣一次進樣可以實現環境空氣中117組分的檢測,但是罐體本身的吸附會影響檢測結果的準確性。 

    關鍵詞:蘇瑪罐;直接進樣;GC-FID-MS;117 VOCs

    中圖分類號:0657.71      文獻標識碼:A      文章編號:0258-32832022--

     

    Comparison of the Determination of 117 Component VOCs Simultaneously Using Online and Canister Sampling Method WANG Xiao, WANG Cheng-ran, LI Zhi-ang, WANG Kai, ZHOU Xin* (National Institute of Measurement and Testing Technology, Chengdu, Sichuan 610021, China), Huaxue Shiji, 2022, 448,~

    Abstract: In this study, a 117 component VOCs standard gas mixture was diluted to 5 nmol/mol and then directly connected to GC-MS with a pre-concentration system (equal to the online sampling method), which was compared to that diluted into a new canister before analyzing by GC-MS (canister sampling method). The result showed that the differences of most components were less than 10% with the relative standard deviation (RSD) between 0.5% ~ and 8%, while a response of formaldehyde through a canister sampling method was significantly 30% lower than the direct sampling method and crotonaldehyde was also declined 12%. Besides, the concentration of formaldehyde decayed by 18% under 60% RH humidity conditions. It is possible to determine 117 component VOCs simultaneously using the canister sampling method but the adsorption should be seriously considered which will influence the accuracy.

    Key words: SUMMA canister; online sampling method; GC-FID-MS; 117 VOCs

    引用本文:王瀟,王成然,李志昂,等.在線監測直接進樣和罐采樣方法一次性分析117組分VOCs的比較[J]. 化學試劑,2022,4481191-1196.

     

     

    基于沸石咪唑酯骨架結構材料11的微固相萃取結合高效液相色譜用于水樣中五種紫外吸收劑的測定

    王穎臻,葛丹丹*,宋家漫,沈茂珍

    (昆明學院 化學化工學院,云南 昆明  650214)

    摘要:建立了一種基于ZIF-11的膜保護微固相萃取μ-SPE的樣品前處理方法,并與高效液相色譜HPLC)聯用測定環境水樣中種紫外吸收劑。對洗脫劑種類、固相萃取劑用量、洗脫時間、萃取時間、鹽濃度、pH值系列影響萃取效率因素的相關條件進行優化。結果表明,固相萃取劑用量10 mg、萃取時間8 min、洗脫劑V(甲醇):V(乙腈)=3:7、洗脫時間9 min、溶液pH7、10 mg/mL氯化鈉條件下,5種紫外吸收劑在5  1000 ng/mL范圍內線性關系良好,相關系數均大于0.992 5,檢出限為0.8  1.5 ng/mL;定量限為2.5 5.0 ng/mL;相對標準偏差為0.9%  6.5%。方法簡單、快速、準確,用于測定湖水、河水、自來水中的紫外線吸收劑,回收率為88.7%  112.3%,相對標準偏差為0.3%  5.5%。

    關鍵字:沸石咪唑酯骨架結構材料-11;漩渦輔助微固相萃取;紫外吸收劑;水樣分析

    中圖分類號:X830    文獻標識碼:A    文章編號:0258-32832022--

     

    Zeolite Imidazolate Framework 11 Based Vortex-Assisted Micro-Solid-Phase Extraction of 5 Kinds of UV Filters in Water Samples Followed by High Performance Liquid Chromatography WANG Ying-zhen, GE Dan-dan, SONG Jia-man, SHEN Mao-zhen (School of Chemistry and Chemical Engineering, Kunming University, Kunming 650214) , Huaxue Shiji,2022,44 (8),00 ~ 00

    Abstract: Zeolite imidazolate framework 11 based micro-solid-phase extraction (μ-SPE), followed by high-performance liquid HPLC with diode array detection method was developed for the determination of 5 kinds of UV filters in water samples. Parameters affecting VA-μ-SPE efficiencies such as extraction sorbent amount, desorption solvent, vortex time, desorption time, solution pH, and salt concentration were investigated. The optimum extraction conditions were as follows: the amount of sorbent was 10 mg, extraction time was 8 min, desorption time was 9 min, desorption solvent was V (methanol) : V (acetonitrile) = 3:7, solution pH was 7 and salt concentration was 10 mg/mL of sodium chloride. Under the optimized conditions, the linearity range was in the range of 51000 ng/mL with correlation coefficients higher than 0.9925. Limits of detection and limits of quantification were in the range of 0.81.5 ng/mL and 2.55.0 ng/mL, respectively. Finally, the proposed method was successfully applied to determine UV filters in real water samples. The relative recoveries ranged from 88.7%112.3%. The developed method proved to be simple, quick, exact, and can be used to determine UV filters in real water samples.

    Keywords: Zeolite imidazolate framework 11; vortex-assisted micro-solid-phase extraction; UV filters; water sample

    引用本文:王穎臻,葛丹丹,宋家漫,等. 基于沸石咪唑酯骨架結構材料11的微固相萃取結合高效液相色譜用于水樣中五種紫外吸收劑的測定[J]. 化學試劑, 2022, 44(8): 1197-1202。

     

     

    氣相色譜-質譜聯用法測定杜仲葉中活性成分肉桂酸

    呂竹茵,陳燕秋,徐增益,肖斌,李猷,雷雯*

    (上?;ぱ芯吭河邢薰?/span> 上海市穩定同位素檢測及應用研發專業技術服務平臺,上海  200062

     

    摘要:肉桂酸作為一種安全性高的活性物質,廣泛用于香精、醫藥以及塑料、樹脂等精細化工產品中。對杜仲葉進行預處理,通過優化凈化條件,利用氣相色譜-質譜聯用法對中草藥杜仲葉中的活性物質肉桂酸的含量進行了準確地定量。結果表明,色譜柱采用Agilent HP-5 MS毛細管柱(30 m×0.25 mm×0.25 μm);載氣為純度為99.999%的高純氦氣;流速為1.0 mL/min;進樣口溫度280 ;分流比為1:50 (體積比);利用多反應監測模式(MRM)采集樣品的質譜信息,該方法檢出限約為0.02 mg/g,定量限為0.07 mg/g,肉桂酸在3個加標濃度下的回收率為80.2%104.6%。開發的檢測方法重現性好、回收率高、精密度高,可為中藥中活性成分的準確定量提供方法參考。

    關鍵詞:氣相色譜-質譜聯用法;肉桂酸;中草藥;杜仲葉;準確定量

    中圖分類號:O658    文獻標識碼:A       文章編號:0258-32832022--

      

    Determination of the Active Ingredient Cinnamic Acid in Eucommia Ulmoides Leaves by Gas Chromatography-Mass Spectrometry LV Zhu-yin, CHEN Yan-qiu, XU Zeng-yi, XIAO Bin, LI You, LEI Wen* (Shanghai Research Institute of Chemical Industry Co, Ltd, Shanghai stable isotope detection and application R & D professional technical service platform, Shanghai 200062, China), Huaxue Shiji, 44(8),

    Abstract: As a safe active substance, cinnamic acid is widely used in flavors, medicines, and fine chemical products such as plastics and resins. In this paper, Eucommia ulmoides leaves were pretreated, and the content of the active substance cinnamic acid in Chinese herbal medicine Eucommia ulmoides leaves was accurately quantified by gas chromatography-mass spectrometry by optimizing the purification conditions. The results show that the column adopts Agilent HP-5 MS capillary column (30 m×0.25 mm×0.25 μm); the carrier gas is high-purity helium with a purity of 99.999%; the flow rate is 1.0 mL/min; the inlet temperature is 280 ; the split ratio was 1:50 (volume ratio); the mass spectrometry information of the sample was collected by the multiple reaction monitoring modes (MRM), the detection limit of the method was about 0.02 mg/g, and the quantification limit was 0.07 mg/g. The recoveries at the three spiked concentrations were 80.2%~104.6%. The detection method developed in this paper has good reproducibility, high recovery rate, and high precision, which can provide a method reference for the accurate quantification of active components in traditional Chinese medicine.

    Key words: gas chromatography-mass spectrometry; cinnamic acid; Chinese herbal medicine; Eucommia ulmoides leaves; accurate quantification

    引用本文呂竹茵,陳燕秋,徐增益,. 氣相色譜-質譜聯用法測定杜仲葉中活性成分肉桂酸[J]. 化學試劑,2022,44(8)1203-1207.

     

     

    基于氧化石墨烯和三鏈DNA的三聚氰胺檢測研究

    張麗媛,范淼,盧宏飛,張廉奉*,邢小靜*

    (南陽師范學院 化學與制藥工程學院,河南 南陽  473061

     

    摘要發展成本低、準確高、特異性好的三聚氰胺檢測方法具有重要的研究意義。基于氧化石墨烯(GO)自身較好的熒光猝滅性能,結合含脫堿基位點的三鏈DNA核酸外切酶III的特殊性能,構建了一種高靈敏的特異性三聚氰胺檢測新方法。首先制備了GO,并采用紫外-可見吸收光譜儀、傅里葉紅外吸收光譜儀及透射電子顯微鏡對其進行了表征。在最佳的實驗條件下,考察了設計方法對三聚氰胺的檢測靈敏度和特異性。結果顯示,體系熒光強度與三聚氰胺濃度呈現較好的線性關系,線性范圍為0.5×10-9 mol/L7.0×10-9 nmol/L,檢測限為0.32×10-9 mol/L。此外,本方法對奶粉樣品中三聚氰胺檢測的回收率為92.8%106.1%,表現出很好的實際應用潛力。

    關鍵詞三聚氰胺;氧化石墨烯;三鏈DNA;脫堿基位點;核酸外切酶III

    中圖分類號O657.3         文獻標識碼:A       文章編號:0258-32832022--

     

    Study on Melamine Detection Based on Graphene oxide and DNA triplex structur ZHANG Li-yuan, FAN Miao, LU Hong-fei, Zhang Lian-feng*, XING Xiao-jing* (College of Chemistry and Pharmaceutical Engineering, Nanyang Normal University, Nanyang 473061, China), Huaxue Shiji, 44(8),

    AbstractIt is of great significance to develop a method for melamine detection with low-cost, high accuracy, and good specificity. Based on the fluorescence quenching property of graphene oxide (GO), combined with the special properties of DNA triplex structure with the abasic site and exonuclease III, a novel platform for melamine detection was developed. GO was first successfully prepared and characterized using UV-visible absorption spectroscopy, Fourier transforms infrared spectroscopy, and transmission electron microscopy. Under the optimum conditions, the detection sensitivity and specificity were investigated. The results showed that the fluorescence intensity displayed a good linear relationship with melamine concentration in the range from 0.5×10-9 mol/L to 7.0×10-9 nmol/L, and the detection limit was 0.32×10-9 mol/L. Moreover, the recovery of melamine spiked in milk powder was from 92.8 % to 106.1%, indicating the potential of the proposed method in practical application.

    Key wordsmelamine; graphene oxide; triplex-stranded DNA; abasic site; exonuclease III

    引用本文:張麗媛,范淼,盧宏飛,等. 基于氧化石墨烯和三鏈DNA的三聚氰胺檢測研究[J]. 化學試劑, 2022, 44(8): 1208-1212。

     

     

    高效液相色譜法測定工業雙酚A中的微量雜質

    黃煜*1 ,李杰2

    1. 中國石油化工股份有限公司 北京化工研究院 標準研究所 北京 100013;2. 上海市計量測試技術研究院 上海 201203

     

    摘要:建立了高效液相色譜法定量分析工業雙酚A中微量雜質的方法。采用C18柱分離,(乙腈:甲醇)-水流動相梯度洗脫,紫外檢測器在280 nm處檢測、內標校正因子法定量。結果表明,在優化的色譜條件下,目標組分的分離度高,線性范圍寬、重復性好,相對標準偏差0.5%2.6%,最低檢測限為0.050.1 mg/kg,5400 ppm加標回收率為103%108%。該方法簡便、高效、準確、靈敏,應用于雙酚A中微量雜質分析,可以滿足工業雙酚A產品質量檢驗需求和生產工藝優化、質量控制中對分析測試方法的需求。

    關鍵詞:高效液相色譜;內標法;工業雙酚A;質量控制

    中圖分類號O656    文獻識別碼A    文章編號0258-32832022--

     

    Determination of Trace Impurities in Industrial Bisphenol A by High Performance Liquid Chromatography HUANG Yu*1, LI Jie2 (1. Institute of standards, Beijing Research Institute of chemical industry, China Petrochemical Corporation, Beijng 100013, China; 2. Shanghai Institute of Metrology and testing technology, Shanghai 201203, China), Huaxue Shiji, 2022, 44(8),

    Abstract: Established a high performance liquid chromatography method for quantitative analysis of trace impurities in industrial bisphenol A. Using C18 (4.6×250 mm×5 μm) column, UV detector, (acetonitrile: methanol)-water as mobile phase, and internal standard correction factor method for quantification. The results show that under the optimized chromatographic conditions, the target components have high resolution, wide linear range and good repeatability, the relative standard deviation is 0.5%2.6%, the minimum detection limit is 0.050.1 mg/kg, the recovery rate of standard addition was 103%108%. The method is simple, efficient, accurate and sensitive. It can be applied to the analysis of trace impurities in bisphenol A, and can meet the needs of quality inspection, production process optimization and quality control for industrial bisphenol A.

    Keywords: high performance liquid chromatography;internal standard method;industrial bisphenol A;quality control

    引用本文黃煜,李杰. 高效液相色譜法測定工業雙酚A中的微量雜質[J]. 化學試劑,2022,4481213-1217.

     

     

    基于穩定同位素質譜技術的進口牛肉產地溯源技術研究

     

    陳庚超,楊雪嬌*,王靜,徐正華,吳思超,郭媛媛,鄭思垳,黃智娟,房小晴,李星穎

    黃埔海關技術中心,廣東 東莞  523000

     

    摘要為有效打擊凍肉走私、保障食品安全,采用元素分析儀-穩定同位素比質譜儀(EA-IRMS)技術建立了不同國家動物源性食品產地溯源方法。系統分析來自歐洲、北美洲、南美洲、大洋洲等不同地區牛肉出口國的樣品中四種穩定同位素的分布,采用方差分析(Analysis of variance,ANOVA)及主成分分析(Principal Component Analysis,PCA),探討了五大地區牛肉樣品中13C、15N、2H、18O等同位素組成的變化規律。結果顯示,來自不同國家的牛肉的δ 13C、δ15N、δ 2H、δ 18O存在顯著差異,其中δ 13C含量主要與養殖飼料植物種類高度相關,δ 15N含量主要受養殖方式及飼料植物類型影響,δ 2Hδ 18O則主要受生長環境及用水的影響。δ 13C、δ15N、δ2Hδ 18O 4項指標綜合分析對不同國家凍肉中的牛肉產地溯源的正確判別率96.5%。建立的牛肉產地溯源方法可為不同國家凍牛肉或轉口牛肉的鑒別提供關鍵技術支撐。

    關鍵詞:動物源性食品;產地溯源;穩定同位素比質譜儀;地域信息;化學計量學分析

     

    Origin traceability of imported beef based on stable isotope ratio mass spectrometry CHEN Geng-chao, YANG Xue-jiao*, WANG Jing, XU Zheng-hua, WU Si-chao, GUO Yuan-yuan, ZHENG Si-hang, HUANG Zhi-juan, FANG Xiao-qing, LI Xing-ying (Technology Center of Huangpu Customs, DongGuan 523000, China), Huaxue Shiji, 2022, 44(8),

    Abstract: To combat the smuggling of frozen meat effectively and ensure food safety, the technology of elemental analyzer stable isotope ratio mass spectrometry (EA-IRMS) was used to establish a method for tracing animal-derived food in different countries in this paper. The distribution of four stable isotopes in samples from five beef exporting countries in Europe, North America, South America, Oceania, and other regions was systematically analyzed. The changes of 13C、15N、2H and 18O isotopic compositions in beef samples from five regions were studied and discussed by analysis of variance (ANOVA) and principal component analysis (PCA). The results show that the δ 13C, δ15N, δ 2H, δ 18O values of beef from different countries have significant differences, among which δ13C content is mainly highly related to the species of cultivated feed plants, δ15N content is mainly affected by breeding methods and feed plant types, while the δ2H and δ18O are mainly affected by the growth environment and drinking water. Based on the comprehensive analysis of δ 13C、δ15N、δ2Hδ 18O, the correct discrimination rate of beef origin traceability in frozen meat from different countries was about 96.5%. The method of beef origin traceability established in this paper can provide key technical support for the identification of frozen beef or entrepot beef from different countries.

    Key words: animal derived food; origin traceability; stable isotope ratio mass spectrometry; regional information; analysis of variance; principal component analysis

    引用本文陳庚超, 楊雪嬌, 王靜, . 基于穩定同位素質譜技術的進口牛肉產地溯源技術研究[J]. 化學試劑, 2022, 44(8): 1218-1223.

     

     

    喹喔啉-2-羧酸標準品的制備與表征

    時若寒1,劉洪斌2,葉子煜2,雷春娟2,韓雪*1,蔡英華*2

    (1. 河北科技大學,河北 石家莊  050018;2. 中國動物疫病預防控制中心,北京  102618)

     

    摘要:根據ISO指南34、35,建立喹喔啉-2-羧酸的有機合成路線并進一步驗證,最終研制出高純度的喹喔啉-2-羧酸標準樣品。通過高效液相色譜、紅外光譜、紫外光譜、質譜、核磁共振光譜的檢測,確定了喹喔啉-2-羧酸的化學結構。研究還使用質量平衡法和定量核磁共振方法聯合定值。并進行了均勻性、短期和長期穩定性的評估和特征值的表征。通過單因素方差分析來獲得合成不確定度。根據質量平衡理論和定量核磁共振方法,確定喹喔啉-2-羧酸純度標準樣品的純度值為:99.5% ± 0.4%,k=2,P=0.95。該標準品純度值很高。在4 條件下,喹喔啉-2-羧酸6個月表現出均勻穩定的特性,可以為我國動物源性產品中關于卡巴氧殘留的檢測標準提供可靠的標樣支撐。

    關鍵詞喹喔啉-2-羧酸;標準物質;穩定性;不確定度

    中圖分類號      文獻標識碼A    文章編號0258-32832022

     

    Preparation and Characterization of a New Reference of Quinoline-2-carboxylic SHI Ruo-han1, LIU Hong-bin2, YE Zi-yu2, LEI Chun-juan2, HAN Xue*1, CAI Ying-hua*2 (1. School of Food and Biology, Hebei University of Science and Technology, Hebei 050018, China; 2. China Animal Disease Prevention and Control Center, Beijing 102618, China) , Huaxue Shiji,2022,44 (8),00 ~ 00

    AbstractAn organic synthesis route of quinoxaline-2-carboxylic acid was established and further verified according to the ISO Guides 34 and 35, and finally a high-purity quinoxaline-2-carboxylic acid reference material was developed. The structure of the compound was determined by the detection of high-efficiency liquid chromatography, infrared spectrum, ultraviolet spectrum, mass spectrum, and nuclear magnetic resonance spectrum. This research used the combined value assignment of the mass balance method and the quantitative NMR, evaluation of homogeneity, and short-term and long-term stability, to characterize the certified value. Homogeneity, short-term and long-term stability, and value characterization are summarized in this research. Uncertainty was obtained according to ANOVA. The purity value of mass balance theory and quantitative NMR method for the reference sample of quinoxaline-2-carboxylate purity was determined as 99.5% ± 0.4%, k=2, p=0.95. At 4  degrees, quinoxaline-2-carboxylic acid was homogenous and stable over 6 months, which can provide reliable sample support for the detection standard of carbadox residue in animal-derived products in China.

    Key words: quinoxaline-2-carboxylic acid; reference material; homogeneity; uncertainty

    引用本文:時若寒,劉洪斌,葉子煜,等. 喹喔啉-2-羧酸標準品的制備與表征 [J]. 化學試劑, 2022, 44(8): 1224-1232。

     

     

    β-硫代糖苷的合成方法研究及晶體結構表征

    華敏1,熊濤1,陳紹彥2,曹燕來2,姚輝1,黃年玉*1,劉明國*1

    (1. 三峽大學 生物與制藥學院天然產物研究與利用湖北省重點實驗室,湖北 宜昌 443002;2. 湖北廣辰藥業股份有限公司,湖北 宜昌 443002)

    摘要:通過化學方法非對映選擇性合成β-硫代糖苷,并對其進行結構分析。以三乙?;咸严┨菫槠鹗荚?,經過水解、縮合、酯化后得到葡萄烯糖-3-吡啶酸酯,篩選了鈷催化下其與苯亞磺酸鈉反應的最佳條件,合成系列β-硫代糖苷衍生物,分析產物的立體化學結構。以三乙?;咸严┨菫槠鹗荚辖?/span>4步反應合成β-硫代糖苷,總率為42%46%;通過X射線單晶衍射分析出(4aR,6S,8aS)-6-((4-氯苯基)硫代)-2-(4-甲氧基苯基)-4,4a,6,8a-四氫吡喃[3,2-d][1,3]Flack參數為0.002(6)。該方法使用廉價金屬催化劑,無毒無臭,操作簡便,為β-硫代糖苷的研究提供理論依據和基礎。

    關鍵詞:鈷催化;硫糖苷;合成;晶體結構;α-葡萄糖苷酶抑制活性

    中圖分類號:R914.5     文獻標識碼:A      文章編號:0258-32832022--

     

    Synthesis and crystal structure characterization of β-thioglycoside HUA Min1, XIONG Tao1, CHEN Shao-yan2, CAO Yan-lai2, YAO Hui1, HUANGNian-yu*1, LIU Ming-guo*1 (1. Key Laboratory of Natural Products Research and Development, College of Biological and Pharmaceutical Sciences, China Three Gorges University,Yichang 443002, Hubei, China;2. Hubei Guangchen Pharmaceutical Co. Ltd, Yichang 443002, Hubei China),Huaxue Shiji, 2022, 44(8),

    Abstract: β-thioglycosides were diastereoselectively synthesized by chemical methods, and their structures were analyzed. The picoloylglucal donor was obtained by hydrolysis, condensation, and esterification from the starting material of commercial tri-O-acetyl-D-glucal. After screening the optimized reaction conditions of picoloylglucal donor and sodium benzene sulfinate, a series of β-thioglycosides was synthesized under the catalysis of cobalt. Then the stereochemical structures of the products were characterized. The β-thioglycosides were synthesized with a total yield of 42%46% by four-step reaction using tri-O-acetyl-D-glucal as the starting material, and compound 5b                                        was analyzed by X-ray crystallography with a Flack parameter of 0.002(6). This simple methodology using cheap, nontoxic, and odorless metal catalysts would provide a theoretical basis for the study of β-thioglycosides.

    Keywords: cobalt catalysis; thioglycoside; synthesis; crystal structure; α-glucosidase inhibitory activity

    引用本文:華敏,熊濤,陳紹彥,等. β-硫代糖苷的合成方法研究及晶體結構表征[J]. 化學試劑,2022,44(8): 1233-1240。

     

     

    新型18F標記的多巴胺正電子發射顯影劑前體的合成

    陳瑜,李如雯,謝樹英,劉中強*

    (海南大學 藥學院,海南 ???/span>  570228

     

    摘要報道了以多巴胺為原料,3種新型18F標記的多巴胺正電子發射顯影劑前體的合成方法。在Boc酸酐的作用下,多巴胺轉化成全保護的中間體,接著單質碘親電取代多巴胺6-位的氫,然后與聯硼酸頻那醇酯發生偶聯反應,得到有機硼酸酯。最后,在雙氧水的作用下,有機硼酸酯水解,羥基取代多巴胺的6-位;采用三氟甲磺?;?/span>(Tf)或對甲基苯磺?;?Ts)發生酯化反應,以56步和43%51%的總產率得到3種芳香環上連有TfTs基團的新型前體化合物。3種新型前體的芳香環上連有易離去基團,有利于親核取代反應,不含重金屬離子及避免了繁瑣的重金屬離子清除步驟,非常適于作為顯影劑前體,為進一步研究氟代多巴胺([18F]FDA)在PD和多種癌癥早期顯像方面的性能提供了基礎。

    關鍵詞:多巴胺;正電子發射顯影劑;前體;合成;帕金森病

     

    Synthesis of the new precursors of 18F-labeled for dopamine used in positron emission tomography CHEN Y, LI Ru-wen, XIE Shu-ying, LIU Zhong-qiang* (School of Pharmacy, Hainan University, Haikou 570228, China), Huaxue Shiji, 2022, 44(8),

    Abstract: Using dopamine as a starting material, the synthesis of three new precursors of 18F-labeled dopamine used in positron emission tomography for tumor imaging was reported. Under the action of Boc anhydride, dopamine was converted into a fully protected intermediate, which was then reacted with iodine electrophilically to replace the hydrogen at position 6 of dopamine. Next, organic borate ester was obtained by coupled with bis (pinacolato) diboron. Finally, under the action of hydrogen peroxide, the organic borate ester was hydrolyzed and the hydroxyl group replaced the 6-position of dopamine. Trifluoromethanesulfonate (Tf) or p-methyl benzenesulfonate (Ts) were esterified to obtain three new precursor compounds with Tf or Ts groups attached to aromatic rings, which went through 56 steps with a total recovery of 43%51%. The aromatic rings of the three new precursors were attached with easy leaving groups, which were conducive to nucleophilic substitution reactions. In addition, without heavy metal ions, they avoided the tedious heavy metal ion removal steps. Given all this, the synthesized three new precursors were very suitable as the developer precursors, providing a basis for further research on the performance of fluorinated dopamine ([18F] FDA) in PD and early imaging of various cancers.

    Key words: dopamine; positron emission developer; precursor; synthesis; Parkinson's disease

    引用本文:陳瑜,李如雯,謝樹英,等. 新型18F標記的多巴胺正電子發射顯影劑前體的合成[J]. 化學試劑,2022,44(8): 1241-1247。

     

    2022化學試劑第8期PDF文檔.pdf

     

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