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DOI10.3724/SP.J.1123.2019.04005
Determination of 11 sulfonamides in pork by two-step liquid-liquid extraction-solid phase extraction purification coupled with high performance liquid chromatography-tandem mass spectrometry
Liu Peiyong; Zhang Hui; Mi Zhijin; Zhang Liangcheng; Zhang Guangren
通讯作者Liu, PY
来源期刊CHINESE JOURNAL OF CHROMATOGRAPHY
ISSN1000-8713
出版年2019
卷号37期号:10页码:1098-1104
英文摘要A method based on two-step liquid-liquid extraction-solid phase extraction purification coupled with high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of 11 common sulfonamides in pork. The samples were extracted first with ethyl acetate containing 2% (v/v) formic acid and then with acetone for the second step. The supernatant was degreased with n-hexane and cleaned using an Oasis MCX SPE column. Finally, nitrogen was blown over the obtained mixture, and the mixture was filtered for conducting HPLC-MS/MS analysis. The sulfonamides were detected in the multiple reaction monitoring positive ion mode, and quantification was performed by employing the external standard method with matrix calibration curves. All the 11 sulfonamides demonstrated good linearity in the range of 20-400 mu g/L, with the correlation coefficient (r(2)) higher than 0.99. The limits of detection (LODs; S/N = 3) and limits of quantification (LOQs; S/N = 10) were found to be in the ranges of 0.1 - 1.0 mu g/kg and 0.2 - 3.0 mu g/kg, respectively. Furthermore, the results indicated that the average recoveries of the 11 sulfonamides ranged from 79.3% to 105.5% at three spiked levels of 50, 100, and 200 mu g/kg, with the relative standard deviations (RSDs) in the range of 1.3% - 11.6% (n = 6). This method showed higher extraction efficiency than the one-step liquid-liquid extraction, and the detection sensitivity was highly improved.
英文关键词high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) two-step liquid-liquid extraction solid phase extraction (SPE) sulfonamides veterinary drug residues pork
类型Article
语种中文
收录类别ESCI
WOS记录号WOS:000502590800011
WOS类目Chemistry, Analytical
WOS研究方向Chemistry
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/333983
作者单位[Liu Peiyong; Zhang Hui; Mi Zhijin; Zhang Liangcheng; Zhang Guangren] Dazhou Food & Drug Inspect Inst, Dazhou 635000, Peoples R China
推荐引用方式
GB/T 7714
Liu Peiyong,Zhang Hui,Mi Zhijin,et al. Determination of 11 sulfonamides in pork by two-step liquid-liquid extraction-solid phase extraction purification coupled with high performance liquid chromatography-tandem mass spectrometry[J],2019,37(10):1098-1104.
APA Liu Peiyong,Zhang Hui,Mi Zhijin,Zhang Liangcheng,&Zhang Guangren.(2019).Determination of 11 sulfonamides in pork by two-step liquid-liquid extraction-solid phase extraction purification coupled with high performance liquid chromatography-tandem mass spectrometry.CHINESE JOURNAL OF CHROMATOGRAPHY,37(10),1098-1104.
MLA Liu Peiyong,et al."Determination of 11 sulfonamides in pork by two-step liquid-liquid extraction-solid phase extraction purification coupled with high performance liquid chromatography-tandem mass spectrometry".CHINESE JOURNAL OF CHROMATOGRAPHY 37.10(2019):1098-1104.
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