降血糖类保健食品中非法添加的8种药物检测及实例分析

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降血糖类保健食品中非法添加的8种药物检测及实例分析

黄湘鹭,王静文,曹进,张庆生

中国食品药品检定研究院

收稿日期:2013-09-12 修回日期:2014-05-08 出版日期:2014-05-25 发布日期:2014-05-29
通讯作者: 黄湘鹭 E-mail:xianglu_huang@126.com
基金资助:
利用酪蛋白胶束-乳铁蛋白动态包裹-释放机制开发活性乳铁蛋白的集成膜过滤技术

Detection of 8 drugs in antidiabetic supplements and Case’s study

Received:2013-09-12 Revised:2014-05-08 Online:2014-05-25 Published:2014-05-29

摘要/Abstract

摘要： 目的建立检测降血糖类保健食品中非法添加8种药物的方法并用于实际检测。方法采用高效液相色谱-串联质谱（HPLC-MS/MS）法，以ZORBAX Eclipse Plus C18(2.1×50mm,1.8μm)色谱柱，以0.1%甲酸溶液为流动相A，甲醇为流动相B，梯度洗脱。通过分子离子峰、二级碎片、色谱保留时间等信息，对宣称辅助降血糖类保健食品非法添加8种化学药物进行鉴别和定量测定。结果：8种药物实现了同时分离与专属鉴定，检出限为0.031～0.15 ng/mL，精密度为1.15%～4.30%，回收率74.0%～109.6%；本法适用于硬胶囊样品；利用本法，从15批样品中检测出9批含非法添加化学药物。结论：本方法专属性强、灵敏度高，结果准确可靠，可作为宣称辅助降血糖类保健食品中检测非法添加化学药物的方法参考。

关键词: 高效液相色谱-串联质谱法, 降糖药物, 格列本脲, 西地那非

Abstract: Objective To develop a method for the identification of 8 drugs in antidiabetic supplements that could be used in practices. Methods The chromatography was performed using a ZORBAX Eclipse Plus C18 column(2.1×50mm,1.8μm), with the mobile phase of 0.1% formic acid(phase A) and methanol(phase B) by gradient elution. 8 illegal syntheic drugs in antidiabetic healthy food were determined qualitatively and quantitatively by the information of the molecular ion mass and specific fragment ions and chromatographic retention. Results 8 drugs could be separated and identificated simltaneously. The limit of detection of these substance was 0.031～0.15 ng/mL, the precision was 1.15%～4.30% and the standard addition recoveries were in the range of 74.0%～109.6%. The method was suitable for the hard capsules. In the 15 batches of samples, illegal syntheic drugs were found in 9 batches. The Conclusion The method was proved to be simple, sensitive and accurate, which could be used as an reference in the detection of illegal synthetic drugs in antidiabetic supplements.

Key words: high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS), antidiabetics, Glibenclamide, Sildenafil

中图分类号:

R917

黄湘鹭王静文曹进张庆生. 降血糖类保健食品中非法添加的8种药物检测及实例分析[J]. 食品科学, 0, (): 0-0.

参考文献

[1] 保健食品注册管理办法（试行）[S].国家食品药品监督管理局令第19号，2005. [2]荫士安, 王茵.试论保健食品的安全性[J].中华预防医学杂志, 2006, 40(2):141-143 [3]王兰明.我国食品安全管理工作的现状与思考[J].食品科学, 2004, 25(7):187-192 [4]孙鑫贵, 李春雨, 赵榕.保健食品违法添加药物状况及管理对策[J].首都公共卫生, 2010, 4(004):153-155 [5]董永成, 杜士明, 陈永顺, 等.中成药及保健品非法添加化学成分的类型, 危害及对策[J].时珍国医国药, 2006, 17(8):1601-1602 [6]汤文璐, 王永铭, 杜文民.国内年文献源抗糖尿病药物的不良反应分析[J].中国新药与临床杂志, 2002, 21(12):753-758 [7]柯俊, 汤文璐.年上海市口服抗糖尿病药物的不良反应报告分析[J].中国临床药学杂志, 2011, 20(6):351-356 [8]Turner R C, Holman R R, Cull C A, et al.Intensive blood-glucose control with sulphonylureas or insulin compared with conventional treatment and risk of complications in patients with type 2 diabetes (UKPDS 33)[J].lancet, 1998, 352(9131):837-853 [9]陈婕.口服抗糖尿病药物不良反应报告分析[J].海峡药学, 2012, 24(3):250-250 [10]Boolell M, Allen M J, Ballard S A, et al.Sildenafil: an orally active type 5 cyclic GMP-specific phosphodiesterase inhibitor for the treatment of penile erectile dysfunction[J].International journal of impotence research, 1996, 8(2):47-52 [11]Rendell M S, Rajfer J, Wicker P A, et al.Sildenafil for treatment of erectile dysfunction in men with diabetes[J].JAMA: the journal of the American Medical Association, 1999, 281(5):421-426 [12]郭应禄, 朱积川, 潘天明, 等.口服西地那非治疗勃起功能障碍疗效和安全性的临床研究[J].中华泌尿外科杂志, 2001, 22(7):389-394 [13]沈周俊, 余燕岚.型磷酸二酯酶抑制剂治疗勃起功能障碍的疗效和安全性[J].中华男科学杂志, 2005, 11(8):631-634 [14]Dalan R，Leow MK，George J，et al．.Neuroglycopenia and adrenergic responses to hypoglycaemia：insights from a local epidemic of 5erendipitous massive overdose of glibenclamide．[J].CKabet med．, 2009, 26:105-109 [15] Poon wT，Lam YH，Lee HH，et aI．.outbreak of hypoglycemia：Sexual enhancement products containing oral hypogIycaemic agent．[J].Hong Kong Med J, 2009, :196-200 [16]邓正照，李琳，卢齐等.非法壮阳药与低血糖[J].中国糖尿病杂志, 2011, 19(2):83-84 [17]Dey J，Shepherd MD.Evaluation and treatment of erectile dysfunction in men with diabetes mellitus[ J ][J].Mayo Clin Proc, 2002, 77(3):276-282 [18]Alberti K G M M, Zimmet P Z.Definition,diagnosis and classification of diabetes mellitus and its complicationsPart 1: diagnosis and classification of diabetes mellitus. Provisional report of a WHO consultation[J].Diabetic medicine, 1998, 15(7):539-553 [19]Hakim L S, Goldstein I.Diabetic sexual dysfunction[J].Endocrinology & Metabolism Clinics of North America, 1996, 25(2):379-400 [20] 现代糖尿病学[M].上海医科大学出版社, 復旦大学出版社, 2000.

降血糖类保健食品中非法添加的8种药物检测及实例分析

Detection of 8 drugs in antidiabetic supplements and Case’s study

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