Rapid Screening of 10 Illegally Adulterated Androgen Drugs in Health Foods by High Performance Liquid Chromatography-Quadrupole-Time-of-flight Mass Spectrometry
  
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KeyWord:high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry  androgen drugs  rapid screening  health food
  
AuthorInstitution
ZHANG Hong-yan,QIU Guo-yu,SHI Xiao-feng,WANG Xing-zhi,WANG Xiao-qiao,XU Xiao-hui,LI Chen-xi,PAN Xiu-li 1.Lanzhou Institute for Food and Drug Control;2.Gansu Province Academy of Medical Sciences
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Abstract:
      An analytical method was established for the determination of 10 illegally adulterated androgen drugs in health foods by high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry(HPLC-Q-TOF MS).The samples were extracted by ultrasonic cleaning or liquid-liquid extraction.10 androgen drugs were separated on a C18 column(3.0 mm×150 mm,1.8 μm) by gradient elution with 0.1%(by volume) formic acid containing 10 mmol/L ammonium acetate and 0.1% formic acid acetonitrile,and determined by HPLC-Q-TOF MS.A data base of the accurate molecular mass and a library containing the 10 androgen drugs were established.An automatic retrieval towards the detected results was carried on according to the characteristics of the compound,such as accurate mass,retention time,isotopic ratio and MS/MS spectrum in order to carry out a rapid qualitative analysis.Results showed that 10 androgen drugs had good linear relationships in the concentration range of 2-500 ng/mL with correlation coefficients(r2) greater than 0.999.The limits of detection(LOD) for 10 androgen drugs in three kinds of matrixes were in the range of 0.01-0.06 mg/kg,while the limits of quantitation(LOQ) were 0.03-0.2 mg/kg.The average recoveries for 10 androgen drugs ranged from 74.3% to 113% with relative standard deviations(RSD) of 1.2%-7.7%.Using library search function to rapid screen, which is efficient,sensitive and accurate,the method is suitable for rapid screening of 10 illegally adulterated androgen drugs in health foods.
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