食品科学

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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   

  1. 中国食品药品检定研究院,北京 100050
  • 出版日期:2014-05-25 发布日期:2014-05-29
  • 基金资助:

    “十二五”国家科技支撑计划项目(2012BAK08B02)

Determination of 8 Drugs in Antidiabetic Supplements: A Case Study

HUANG Xiang-lu, WANG Jing-wen, CAO Jin, ZHANG Qing-sheng   

  1. National Institutes of Food and Drug Control, Beijing, 100050, China
  • Online:2014-05-25 Published:2014-05-29

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-串联质谱法,以ZORBAX Eclipse Plus C18(2.1 mm×50 mm,1.8 μm)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5.5~76 ng/g,精密度为0.22%~1.19%,回收率为74.0%~111.9%;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 and apply a method for the identification of 8 illegal drugs in antidiabetic supplements
using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS). Methods: The chromatography
was performed using a ZORBAX Eclipse Plus C18 column (2.1 mm × 50 mm, 1.8 μm), with a mobile phase consisting of
0.1% (V/V) formic acid (phase A) and methanol (phase B) by gradient elution. Eight illegal synthetic drugs (gliquidone,
glibenclamide, glimepiride, sildenafil, repaglinide, glipizide, tadalafil and gliclazide) added in antidiabetic health foods
were determined qualitatively and quantitatively based on the information of molecular ion mass, specific fragment ions and
chromatographic retention. Results: Eight drugs could be separated and identified simultaneously. The limits of detection
(LODs) of these substances were in the range of 5.5–76 ng/g, the precision expressed as relative standard deviation (RSD)
for six replicate determinations was 0.22%–1.19%, and the recoveries from spiked samples were in the range of 74.0%–
111.9%. The method was suitable for hard capsules. In the 15 batches of samples, the illegal synthetic drugs were found in 9
batches. Conclusion: The method has been proved to be simple, sensitive and accurate, and can be used as a reference in the
detection of the illegal synthetic drugs in anti-diabetic supplements.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS), antidiabetics, glibenclamide, sildenafil

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