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刊物信息
期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
编辑部主任:粟晓黎
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237

 

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LC-MS法鉴定桑叶中生物碱类成分

Identification and characterization of alkaloids in mulberry leaf by hyphenated LC-MS techniques

分类号:
出版年·卷·期(页码):2016,36 (10):0-0
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立LC-MS法对桑叶中生物碱类成分进行结构鉴定。方法:对桑叶中生物碱类成分分别采用9-芴甲氧羰酰氯(FMOC-Cl)衍生化后ODS柱分离或Hypersil SCX色谱柱直接分离,电喷雾正离子化高分辨TOF/MS检测,结合MS/MS法和对照品对照法进行鉴定。结果:在所建立的条件下,共检测并鉴定4个生物碱成分(2-氧-α-D-半乳吡喃糖苷-1-脱氧野尻霉素、1-脱氧野尻霉素、荞麦碱和1,4-二脱氧-l,4-亚胺基-D-阿拉伯糖醇),衍生化法和直接测定法2种分离分析方法的鉴定结果相互验证。此外,9-芴甲氧羰酰氯(FMOC-Cl)柱前衍生化法亦适用于桑叶生物碱成分的准确定量,方法准确可靠。结论:桑叶中生物碱类成分鉴定为相关中药的物质基础研究和质量控制提供依据。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To develop a hyphenated LC-MS method for the separation and characterization of alkaloids in mulberry leaf. Methods: The alkaloids were separated on a reversed-phase ODS column after 9-fluorenylmethyl chloroformate pre-column derivatization or Hypersil SCX column by direct cation exchange, respectively. The determination was performed with positive ESI high-resolution TOF-MS of their protonated adduct ions and then the corresponding product mass spectra by tandem mass spectroscopy. The structures of the alkaloids were elucidated afterwards and verified further through reference substances. Results: Four alkaloids(2-O-α-D-galactopyranosyl-1-deoxynojirimycin,1-deoxynojirimycin,fagomine and 1,4-dideoxy-1,4-imino-D-arabinitol)were detected and identified. The results of the two different methods:pre-column derivatization and direct cation exchange were in good agreement. In addition,the method of 9-fluorenylmethyl chloroformate pre-column derivatization,which is accurate and reliable,can also be applied to the quantitation of alkaloids in mulberry leaf. Conclusion: The identification and characterization of the alkaloids in mulberry leaf would provide reference for the quality control and clinical rational of the related traditional Chinese medicines.

-----参考文献:---------------------------------------------------------------------------------------
[1] 中国药典2015年版. 一部[S].2015:297 ChP 2015. Vol Ⅰ[S]. 2015:297
[2] 江苏新医学院.中药大辞典. 下册[M]. 上海:上海科学技术出版社,1997:182 Jiangsu New Medical College. Traditional Chinese Medicine Dictionary. Volume 2[M]. Shanghai:Shanghai Science and Technology Publishers,1997:182
[3] 欧阳臻,陈钧.桑叶的化学成分及其药理作用研究进展[J].江苏大学学报:自然科学版,2003,24(6):39 OU YZ,CHEN J. Research progress on chemical constituents and pharmacological activities of Mulberry Leaves[J]. J Jiangsu Univ: Nat Sci Ed,2003,24(6):39
[4] 徐健飞,义祥辉,陈全斌.桑叶不同化学成分的降血糖作用[J]. 广西植物,2010,30(2):284 XU JF,YI XH,CHEN QB. Effect of different chemical compositions from mulberry leaf on decreasing glucose in blood[J]. Guihaia, 2010,30(2):284
[5] 杨雨,欧阳臻,常钰,等.桑叶不同组分降血糖作用研究[J].食品科学,2007,28(8):454 YANG Y,OUY Z,CHANG Y,et al. Study on hypoglycemic effects of components in mulberry leaves[J]. Food Sci,2007,28(8):454
[6] 张军,宛晓春,陆翠珍,等.桑叶生物碱类化合物的研究进展[J]. 安徽农业大学学报,2012,39(6):993 ZHANG J,WAN XC,LU CZ,et al. The research progress of sugarmimic alkaloids in mulberry[J]. J Anhui Agric Univ,2012,39(6): 993
[7] ZHANG Y,REN C,LU G,et al. Purification,characterization and anti-diabetic activity of a polysaccharide from mulberry leaf[J]. Regul Toxicol Pharm,2014,70(3):687
[8] 何羡霞,苏楠,吴新荣.桑叶降糖有效部位及其降糖活性研究进展[J].中国实验方剂学杂志,2014,20(7):245 HE XY,SU N,WU XR. Research progress of hypoglycemic effective parts and hypoglycemic activity of mubeery leaves[J]. Chin J Exp Tradit Med Form,2014,20(7):245
[9] ASANO N,YAMASHITA T,YASUDA K,et al. Polyhydroxylated alkaloids isolated from mulberry trees(Morus alba L.)and silkworms(Bombyx mori L.)[J]. J Agric Food Chem,2001,49(9):4208
[10] HIRAYAMA C,KONNO K,WASANO N,et al. Differential effects of sugar-mimic alkaloids in mulberry latex on sugar metabolism and disaccharidases of Eri and domesticated silkworms:enzymatic adaptation of Bombyx mori to mulberry defense[J]. Insect Biochem Mol Biol,2007,37(12):1348
[11] 丁俊男,郑桂英,张秀丽,等.北方桑树中1-脱氧野尻霉素含量的测定[J].实验室研究与探索,2012,31(1):12 DING JN,ZHENG GY,ZHANG XL,et al. Determination of 1-DNJ content of northern mulberry varieties[J]. Res Explor Lab,2012, 31(1):12
[12] KIM JW,KIM SU,LEE HS,et al. Determination of 1-deoxynojirimycin in Morus alba L. leaves by derivatization with 9-fluorenylmethyl chloroformate followed by reversed-phase high-performance liquid chromatography[J]. J Chromatogr A,2003,1002(1-2):93
[13] NUENGCHAMNONG N,INGKANINAN K,KAEWRUANG W,et al. Quantitative determination of 1-deoxynojirimycin in mulberry leaves using liquid chromatography-tandem mass spectrometry[J]. J Pharm Biomed Anal,2007,44(4):853
[14] NAKAGAWA K,OGAWA K,HIGUCHI O,et al. Determination of iminosugars in mulberry leaves and silkworms using hydrophilic interaction chromatography-tandem mass spectrometry[J]. Anal Biochem,2010,404(2):217

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