Simultaneous Determination of 72 Veterinary Drugs in Shrimp by Modified QuEChERS and High Performance Liquid Chromatography-Tandem Mass Spectrometry
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Simultaneous Determination of 72 Veterinary Drugs in Shrimp by Modified QuEChERS and High Performance Liquid Chromatography-Tandem Mass Spectrometry
Vol. 31, Issue 5, Pages: 552-558(2012)
作者机构:
1. 河北大学化学与环境科学学院
2. 中国检验检疫科学研究院
3. 燕山大学环境与化学工程学院
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Simultaneous Determination of 72 Veterinary Drugs in Shrimp by Modified QuEChERS and High Performance Liquid Chromatography-Tandem Mass Spectrometry. [J]. 31(5):552-558(2012)
DOI:
Simultaneous Determination of 72 Veterinary Drugs in Shrimp by Modified QuEChERS and High Performance Liquid Chromatography-Tandem Mass Spectrometry. [J]. 31(5):552-558(2012)DOI:
Simultaneous Determination of 72 Veterinary Drugs in Shrimp by Modified QuEChERS and High Performance Liquid Chromatography-Tandem Mass Spectrometry
A method was developed for the simultaneous determination of 72 veterinary residues in shrimps by QuEChERS and high performance liquid chromatography-tandem mass spectrometry.The sample was extracted with 5%acetic acid-acetonitrile,and the supernatant liquid was directly purified with C18,meanwhile,acetonitrile was used for the precipitation of protein.The extract was evaporated under nitrogen stream,and redissolved with 1 mL 0.1%formic acid-acetonitrile(4∶1).Prior to the injection into LC-MS/MS,the sample was filtered through a 0.22 μm filter membrane.The HPLC separation was performed on ZORBAX SB-C18 column by gradient elution with acetonitrile and 0.1%formic acid as mobile phase.The analysis of target compounds was carried out with electrospray ionization(ESI) under multi reaction monitoring(MRM) mode.The external standard method was used for quantification. Under the optimal conditions,the correlation coefficients for 97.2%of the veterinaries were larger than 0.95 in the linear range of 0.1-1 840 μg/kg,the limits of quantitation ranged from 0.02 μg/kg to 33.58 μg/kg.The recoveries of 72 veterinary at three spiked levels were between 61%and 119%,except that for dibutylsuccinate,cefapirin,cefquinome,ceftiofur,lincomycin ane diazinon were between 38%and 58%,and their relative standard deviations were in the range of 1.6%-20%.The established method was used for the screening and determination of real samples(pteris shrimp,freshwater shrimp and sea shrimp) bought from supermarket.It was shown that no residue was detected in the sea shrimp and pteris shrimp samples,and 4.0 μg/kg of sulfadiazine as well as 2.2 μg/kg of sulfamethoxazole were found in freshwater shrimp sample,but the concentrations were all lower than the MRLs.
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