Citation: XU Sen, LI Xiuqin, LUO Ximing, ZHANG Qinghe. International comparison APMP. QM-S6: determination of clenbuterol in porcine meat by isotopic dilution mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(10): 1104-1110. doi: 10.3724/SP.J.1123.2014.06024 shu

International comparison APMP. QM-S6: determination of clenbuterol in porcine meat by isotopic dilution mass spectrometry

XU Sen ^1,2 ,
LI Xiuqin ^1,, ,
LUO Ximing ² ,
ZHANG Qinghe ¹

1.
1. National Institute of Metrology, Beijing 100029, China;

Corresponding author: LI Xiuqin,
Received Date: 16 June 2014

Fund Project: 北京市科技计划课题(Z141100002614009) (Z141100002614009)国家公益性行业科研专项经费项目(2012104010-5) (2012104010-5)国家重大科学仪器装备专项(2012YQ09016703). (2012YQ09016703)

A method was developed for the determination of clenbuterol in porcine meat by isotopic dilution mass spectrometry (IDMS). National Institute of Metrology of China (NIM) participated in the international comparison activity organized by Asia Pacific Metrology (APMP) and got an international mutual recognition result using this method. The important factors of the method, such as the spray voltage, mobile phase, chromatographic column, extraction, purification and filtration conditions were investigated to acquire optimum conditions. The optimization results showed that the composition and pH value of the mobile phase had effects on the response of the mass spectrum of clenbuterol and the optimal value of the spray voltage. The solvent of sample had influences on the chromatographic retention behavior of clenbuterol. It was found that methanol caused a serious solvent effect, even made chromatographic peak split. Since clenbuterol was easily adsorbed on hydrophilic filter membranes and solid phase extraction columns, there were interference suppressions for the quantification of clenbuterol because of the eluate of the solid phase extraction columns. The homogenate method with extraction solvent of 0.1% (v/v) formic acid in acetonitrile had the highest extraction efficiency. The limit of the detection (LOD, S/N>3) of the method was 0.2 μg/kg. The determination results of clenbuterol in the porcine meat by this method were 5.18 μg/kg±0.50 μg/kg (k=2). This method is accurate, reliable, reproducible, and suitable for the determination of clenbuterol with trace quantity in porcine meat.
- isotopic dilution mass spectrometry (IDMS),
- clenbuterol,
- porcine meat,
- international comparison
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