FOOD SCIENCE ›› 2012, Vol. 33 ›› Issue (8): 252-255.doi: 10.7506/spkx1002-6630-201208056

• Analysis & Detection • Previous Articles     Next Articles

Determination of Thirteen Sedative Residues in Meat by Matrix Solid Phase Dispersion-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

QU Yan1,LU Yong2,FENG Nan2,ZHAO Jun-ping2,JIN Wei-wei1,WANG Gui-shuang1   

  1. (1. Beijing Food Brewing Institute, Beijing 100050, China; 2. Beijing Municipal Center for Food Safety Monitoring, Beijing 100041, China)
  • Online:2012-04-25 Published:2012-03-31

Abstract: A matrix solid phase dispersion (MSPD) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method has been developed for the simultaneous determination of alprazolam, midazolam, triazolam, estazolam, oxazeoam, diazepam, nitrazepam, clonazepam, carbamazepin, lidocaine, phenobarbita, amobarbital and secobarbita residues in meat. Sample extract was cleaned up using an MSPD kit before UPLC-MS/MS. The analytes were monitored under multi-reaction monitoring (MRM) mode and quantified by an external standard method. The chromatographic separation was achieved on a BEH C18 column using a mobile phase composed of 10 mmol/L ammonium acetate and methanol through gradient elution. The results showed that the limits of detection for 13 sedatives ranged between 0.05 and 3 μg/kg. The average spike recoveries for the sedatives in a blank pork sample at three spike levels were 77.4%-100.2% with relative standard deviation (RSD) of 1.3%-14.8% (n =3). The method was simple, rapid, sensitive, accurate and applicable for the determination of 13 sedative residues in meat.

Key words: sedative drug, ultra performance liquid chromatography-tandem mass spectrometry, matrix solid phase dispersion (MSPD), meat

CLC Number: