Determination of drug residues in food andbiological samples by using QuEChERS combinedwith liquid chromatography-tandem massspectrometry

• Main Authors: Pei-Cheng Wang, 王培成
• Other Authors: Maw-Rong Lee
• Format: Others
• Language: zh-TW
• Published: 2014
• Online Access: http://ndltd.ncl.edu.tw/handle/15865556598866114816

博士 === 國立中興大學 === 化學系所 === 102 === The aim of this study is to investigate a quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation method coupled with liquid chromatography tandem-mass spectrometry (LC-MS/MS) for trace analysis of drugs residues in food and biological samples. The first part of this study was to develop a rapid and sensitive method for the simultaneous detection of cyromazine and melamine in chicken eggs using the QuEChERS method coupled with LC-MS/MS. The optimal extraction solvent for the liquid-liquid extraction was 5 mL of acetonitrile with a 0.1M hydrochloric acid aqueous solution (99.5 : 0.5, v/v). The extract was cleaned with 0.5 g of anhydrous magnesium sulfate and 10 mg of graphitized carbon black. The detection limits were 1.6 ng g-1 for cyromazine and 8 ng g-1 for melamine, and the quantitation limits were 5.5 ng g-1 for cyromazine and 25 ng g-1 for melamine. The recoveries of cyromazine and melamine in the spiked egg samples were 83.2% and 104.6%, respectively, with an relative standard deviation (RSD) of less than 18.1%. The intra-day and inter-day precisions, represented by the RSD ranged from 1.5% to 8.8% and 6.8% to 14.3%, respectively. The proposed method was tested by analyzing chicken eggs from the markets and from the veterinary medicine laboratory. The concentrations of cyromazine and melamine detected in these samples were in the range of 20 to 94 ng g-1. The results demonstrated that the QuEChERS method combined with LC-MS/MS is a simple, rapid and inexpensive method for the analysis of cyromazine and melamine in eggs. The second part was to develope a fast screening and high-throughput method for the analysis of mulitclassed illicit drugs in human urine by using QuEChERS coupled with LC-HESI-MS/MS. The target illicit drugs are including stimulants, hallucinogens, opioids, benzodiazepines, dissociative anesthetics, and new synthetic cannabinoids. The optimal conditions of the QuEChERS extraction method consisted of 2 mL of acetonitrile with 0.5 g sodium acetate and 5 mg C18-modified silica in 1mL urine sample. The limits of detection and quantification ranged from 0.01 to 2.7ng mL-1 and from 0.03 to 9 ng mL-1, respectively. The recoveries of the illicit drugs ranged from 74% to 117%, with a relative standard deviation (RSD) less than 16%. The RSD of intra- and inter-day precisions ranged from 0.3% to 16% and 0.7% to 20%, respectively. The proposed method was tested by analysis of suspected urine samples from a drug-testing laboratory. The concentrations of the detected illicit drugs ranged from 7 to 14460 ng mL-1. The results demonstrated that the QuEChERS method combined with LC-MS/MS is a simple, rapid, and inexpensive technique for the detection and analysis of illicit drugs in human urine.