Chinese Journal of Chromatography ›› 2015, Vol. 33 ›› Issue (4): 371-376.DOI: 10.3724/SP.J.1123.2014.11020

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Rapid screening and quantitative detection of 11 illegally added antidiabetics in health care products by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

DU Yanshan, LI Qiang, WU Chunmin, ZHANG Yan   

  1. Hebei Food Inspection and Research Institute, Hebei Food Safety Key Laboratory, Shijiazhuang 050091, China
  • Received:2014-11-14 Revised:2015-01-15 Online:2015-04-08 Published:2015-03-30

Abstract:

A method for rapid screening and quantification of 11 antidiabetics (nateglinide, pioglitazone hydrochloride, gliquidone, gliclazide, glipizide, glibenclamide, metformin hydrochloride, repaglinide, phenformin hydrochloride, rosiglitazone hydrochloride, glimepiride) illegally added in health care products by ultra performance liquid chromatography (UPLC)-quadrupole/electrostatic field orbitrap mass spectrometry was established. The samples were extracted with methanol, and separated on an Agilent Poroshell 120 SB-C18 column (100 mm×4.6 mm, 2.7 μm) with acetonitrile-10 mmol/L ammonium acetate solution as mobile phases by gradient elution. The positive mode was used in the MS detection. The resolution of the precursor mass was 70000, while the resolution of the product mass was 17500. The results indicated that the linearity of all the 11 antidiabetics ranged from 0.005 mg/L to 0.5 mg/L with the correlation coefficients greater than 0.99. The limits of detection were confirmed by spiked samples, and were between 2.7 and 5.1 μg/kg for the 11 antidiabetics. The recoveries were in the range of 87.3% to 98.3%, with the relative standard deviations in the range of 2.18%-5.21%. This method is accurate, simple and rapid, and can be used in rapid screening and quantitative analysis of the 11 illegally added antidiabetics in health care products.

Key words: antidiabetics, health care products, quadrupole/electrostatic field orbitrap high resolution mass spectrometry, ultra performance liquid chromatography (UPLC)

CLC Number: