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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

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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