Citation: LIU Yun, DING Tao, LIAO Xue-Qing, SHEN Chong-Yu, JIANG Shan, LV Chen, GUI Qian-Wen, LIU Han, FEI Xiao-Qing, WU Bin, ZHANG Rui, WANG Yan, JI Mei-Quan, WANG Xu-Lu, HUANG Zhi-Qiang. Direct Determination of 42 Chemical Drugs Illegally Added in Herbal Medicines and Dietary Supplement by High Performance Liquid Chromatography-Quadrurpole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(3): 423-429. doi: 10.11895/j.issn.0253-3820.150726 shu

Direct Determination of 42 Chemical Drugs Illegally Added in Herbal Medicines and Dietary Supplement by High Performance Liquid Chromatography-Quadrurpole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry

LIU Yun ,
DING Tao ^1,, ,
LIAO Xue-Qing ² ,
SHEN Chong-Yu ¹ ,
JIANG Shan ¹ ,
LV Chen ³ ,
GUI Qian-Wen ¹ ,
LIU Han ¹ ,
FEI Xiao-Qing ¹ ,
WU Bin ¹ ,
ZHANG Rui ¹ ,
WANG Yan ¹ ,
JI Mei-Quan ¹ ,
WANG Xu-Lu ¹ ,
HUANG Zhi-Qiang ⁴

1.
¹ Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China;
2.
² China Pharmaceutical University, Nanjing 210001, China;
3.
³ Thermol Fisher Scientific, Shanghai 201206, China;
4.
⁴ Hunan Entry-Exit Inspection and Quarantine Bureau, Changsha 410004, China

Corresponding author: DING Tao,
Received Date: 14 September 2015
Available Online: 16 November 2015
Fund Project: 本文系江苏出入境检验检疫局科技计划(No.2015KJ29) (No.2015KJ29)国家科技支撑计划课题(No.2012BAK08B01)基金资助项目 (No.2012BAK08B01)

A method of high performance liquid chromatography-quadrurpole/electrostatic field orbitrap high resolution mass spectrometry (HPLC-Q/Qrbitrap MS) was developed to determine 42 chemical drugs illegally added in herbal medicines and dietary supplements. The samples were pretreated based on the ultrasoni-cassisted extraction by the solvent of methanol-water (6:4, V/V), and centrifuged under 12000 r/min. Subsequently, the solution was filtered by a polytetrafluoroethylene (PTFE) membrane with pore size of 0.22 μm. The analytes were separated on a Phenomenex C₁₈ (100 mm×4.6 mm, 2.6 μm) column through gradient elution with acetonitrile and 0.1% formic acid aqueous solution. The mass spectrometer was operated under Full MS/dd-MS2 experiment using positive and negative mode, respectively. Under the optimal conditions, 42 chemical drugs were well separated. Good linearity was obtained in their respective linear ranges with correlation coefficients higher than 0.99. The average recoveries at three spiked levels (20, 50 and 100 ng/g) were in the range of 69.3%-105.2% and the relative standard deviations (RSDs) lower than 8.9%. Based on the above method, 31 kinds of herbal medicines and dietary supplements were analyzed, in which metformin was found in three samples while sildenafil and hydroxyhomosildenafil were found in one sample, respectively. The proposed method is simple, time saving, high accuracy and sensitive. The method is suitable for confirmation and quantification of 42 chemical drugs in herbal medicines and dietary supplements. The research provides an effective method to control the quality and illegal addition for herbal medical and dietary supplements.
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