| 气相色谱－三重四极杆质谱法测定动物源性食品中砜吡草唑残留量 |
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| 基金项目:福建省科技厅项目（2020Y0075）；厦门海关科技项目（2020XK09）；泉州科技项目（2020N007s） |
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| 中文摘要:建立了动物源性食品中砜吡草唑残留量的气相色谱－三重四极杆质谱检测方法。猪肉、猪肝、鸡肉、鸡肝、牛奶和鸡蛋中的砜吡草唑用乙腈提取，经乙二胺-N-丙基硅烷化硅胶、十八烷基键合硅胶和无水硫酸镁去除杂质，离心后取上清液氮吹至干，加入丙酮复溶、过滤后经气相色谱－三重四极杆质谱检测，外标法定量。通过对仪器条件、提取溶剂和净化方式等进行优化，确定最合适的前处理方法和仪器条件。对样品的基质效应进行考察，发现6种基质中砜吡草唑的基质效应均小于20%，为弱基质效应，无需采取补偿措施。在优化实验条件下，砜吡草唑在0.5 ~ 100 μg/L范围内线性关系良好，相关系数为0.999 5。空白样品在4个加标水平下的平均回收率为85.8% ~ 106%，相对标准偏差（n = 6）为3.1% ~ 6.8%，方法定量下限为0.001 mg/kg。采用该方法对50个动物源性食品进行测定，在1个牛肉样品和1个羊肉样品中检出砜吡草唑。该方法操作简单、灵敏度高、准确性好，适用于动物源性食品中砜吡草唑的检测，可为砜吡草唑在动物源性食品中的风险监控提供技术支撑。 |
| 中文关键词:砜吡草唑 动物源性食品 气相色谱－三重四极杆质谱法 |
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| Determination of Pyroxasulfone Residues in Animal-derived Foods by Gas Chromatography－Triple Quadrupole Mass Spectrometry |
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| Abstract:A gas chromatography－triple quadrupole mass spectrometry was developed for the rapid determination of pyroxasulfone residues in animal-derived foods．Pyroxasulfone residues in pork，pig liver，chicken，chicken liver，milk and eggs were extracted with acetonitrile，and cleaned up with primary-secondary amine，stearyl bonded silica gel and anhydrous magnesium sulfate as dispersive solid-phase extraction sorbent．After centrifugation，the supernatant liquid was nitrogen-blowed to dryness．After redissolved with acetone and filtered，the analyte was detected by gas chromatography－triple quadrupole mass spectrometry，and quantified by external standard method．The instrument conditions，extraction solvents and purification method were optimized in the experiment，and the optimal pretreatment method and instrument conditions were obtained．The detection effects of pyroxasulfone by triple quadrupole liquid chromatography－mass spectrometry and triple quadrupole gas chromatography－mass spectrometry were compared．The results showed that the response of pyroxasulfone on triple quadrupole liquid chromatography－mass spectrometry was poor，and the detection sensitivity could not meet the requirements of relevant regulations，while the detection effect of pyroxasulfone by triple quadrupole gas chromatography－mass spectrometry was excellent，which could meet the detection requirements．In addition，the extraction effects of hexane，acetone，ethyl acetate，acetonitrile and acidic acetonitrile as extraction solvents were compared，and the results showed that acetonitrile was the most suitable extraction solvent．The matrix effect of the sample was investigated，and it was found that the matrix effects of pyroxasulfone in the six matrices were less than 20%，which were a weak matrix effect without compensation. Under the optimal conditions，the calibration curve was linear in the range of 0.5－100 μg/L with correlation coefficients of 0.999 5． The limit of quantitation was 0.001 mg/kg. The average recoveries for blank samples at low，medium and high spiked levels ranged from 85.8% to 106%，with relative standard deviations（n = 6） of 3.1%－6.8%．This method was used to determine 50 animal-derived foods，in which pyroxasulfone residues were detected in one beef sample and one mutton sample．The method is simple，rapid and sensitive，and it could meet the requirements for detection of pyroxasulfone residue in animal-derived foods. |
| Key Words:pyroxasulfone animal-derived foods gas chromatography－triple quadrupole mass spectrometry |
| 引用本文：荣杰峰，张志勇，张松艳，钟坚海，翁城武，乐有东，佘紫文.气相色谱－三重四极杆质谱法测定动物源性食品中砜吡草唑残留量[J].分析测试学报,2022,41(8):1242-1246. |
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