| QuEChERS/液相色谱－串联质谱测定猪肉中赛拉嗪及其代谢产物2，6-二甲基苯胺 |
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| 基金项目:国家重点研发计划（2018YFC1602303）；辽宁省自然科学基金（2020－MS－124） |
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| 中文摘要:建立了QuEChERS/液相色谱－串联质谱测定猪肉样品中赛拉嗪及其代谢产物2，6-二甲基苯胺（DMA）的新方法。样品匀浆后经乙腈－2%乙酸提取、C18吸附剂/N-丙基乙二胺（PSA）净化处理，提取液经氮吹、定容后，以0.1%甲酸－水溶液和0.1%甲酸－乙腈溶液为流动相，采用Waters C18色谱柱（100 mm × 2.1 mm，3.5 μm）进行分离，正离子模式下多反应监测模式检测，基质匹配外标校准曲线定量。赛拉嗪和DMA的线性范围均为0.2～500 μg/L，检出限分别为0.10、0.30 μg/kg，定量下限分别为0.32、1.00 μg/kg，加标回收率分别为95.6%～108%和70.3%～79.5%，相对标准偏差（RSD）分别为2.6%～2.8%和3.1%～5.0%。该方法成功应用于市售猪肉中赛拉嗪和DMA的检测，为肉制品中赛拉嗪和DMA的检测提供了一种简单、快速、灵敏的新方法。 |
| 中文关键词:赛拉嗪 2，6-二甲基苯胺 QuEChERS 液相色谱－串联质谱 猪肉 |
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| Simultaneous Determination of Xylazine and Its Metabolite 2，6-Dimethylaniline in Pork by QuEChERS/Liquid Chromatography－Tandem Mass Spectrometry |
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| Abstract:A novel analytical method for simultaneous determination of xylazine and its metabolite 2，6-dimethylaniline（DMA） in pork was developed based on QuEChERS/liquid chromatography－tandem mass spectrometry（LC－MS/MS）. The analytical process was as follows： pork meat samples were homogenated for 1 min， followed by extraction with acetonitrile－2% acetic acid， cleanup with C18/PSA mixed adsorbent. The extracts were evaporated to dryness with high-purity nitrogen gas， and then dissolved in mobile phase A for LC－MS/MS analysis in positive ionization mode using multiple reaction monitoring（MRM）. The separation was carried out on a Waters C18 separation column（100 mm × 2.1 mm， 3.5 μm） using 0.1% formic acid－water and 0.1% formic acid－acetonitrile as mobile phases. The effects of extraction solvents， types and amounts of adsorbents on the recoveries were investigated. Results showed that the effects of blank matrix on MS response of xylazine and DMA were checked， and the results showed weak suppression effects for xylazine（0.86） and DMA（0.89）. The quantitations of xylazine and DMA were completed by a matrix-matched external calibration method. The limits of detection for xylazine and DMA were 0.10 μg/kg and 0.30 μg/kg， and the limits of quantitation were 0.32 μg/kg and 1.00 μg/kg， respectively.Recoveries for xylazine and DMA were in the ranges of 95.6%－108% and 70.3%－79.5%， with their relative standard deviations（RSD） of 2.6%－2.8% and 3.1%－5.0%， respectively. To validate the developed method， ten pork samples collected from local supermarkets were determined. Xylazine was not detected in the ten samples except for one sample where 1.13 μg/kg of DMA was found. The present method is simple， rapid， sensitive and efficient， and is suitable for the detection of xylazine and DMA residues in pork. |
| Key Words:xylazine 2, 6-dimethylaniline QuEChERS liquid chromatography－tandem mass spectrometry pork |
| 引用本文：张译文，任苏瑜，翟明燕，何 欣，谭 峰.QuEChERS/液相色谱－串联质谱测定猪肉中赛拉嗪及其代谢产物2，6-二甲基苯胺[J].分析测试学报,2021,40(9):1386-1390. |
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