| 表层取样法结合气相色谱－串联质谱测定竹木砧板中19种防腐防霉剂残留 |
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| 基金项目:国家重点研发计划（2017YFC1601806，2017YFC1601805） |
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| 中文摘要:建立了表层取样/气相色谱－串联质谱（GC－MS/MS）测定竹木砧板中19种防腐防霉剂残留的方法。通过表层取样法制备样品后先进行酸化，然后利用乙酸乙酯－正己烷（2∶8，体积比）混合溶剂提取，经方法优化后无需进行衍生化反应及净化操作，采用多反应监测扫描（MRM）模式检测，基质匹配溶液外标法定量。结果表明，19种组分在0.005～200.0 μg/mL范围呈良好的线性关系（r2?> 0.990），检出限（LOD，S/N = 3）为0.001 ~ 0.17 mg/kg，定量下限（LOQ，S/N = 10）为0.003 ~ 0.55 mg/kg；在低、高2个不同加标水平下，19种目标物的回收率为65.8% ~ 97.2%，相对标准偏差（RSD，n = 6）为4.3% ~ 13%。利用该方法对市售竹木砧板和一次性筷子样品进行检测，发现非定型包装竹木砧板中存在五氯酚残留量高的风险隐患，可为相关部门提供风险预警。 |
| 中文关键词:竹木砧板 ?表层取样 ?防腐防霉剂 ?气相色谱－串联质谱 ?风险预警 |
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| Determination of 19 Antiseptic and Antifungal Agents Residues in Wooden Chopping Boards by Gas Chromatography－Tandem Mass Spectrometry with Surface Sampling Method |
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| Abstract:A gas chromatography－tandem mass spectrometry（GC－MS/MS） with surface sampling method was established for the determination of 19 kinds of antiseptic and antifungal agents residues in wooden chopping boards．The samples were prepared by surface sampling method，followed by acidification，and then extracted with ethyl acetate－n-hexane（2∶8，volume ratio） mixed solvent．The optimized method eliminated the need for derivatization reactions and purification operations．Multi-reaction monitoring scanning mode（MRM） was used for monitoring，and the external standard method with matrix-matched solution was used for quantification．Results of the optimized analysis showed that there were good linear relationships for the 19 components in the range of 0.005－200.0 μg/mL，with their correlation coefficients（r2） larger than 0.990．The limits of detection（LODs，S/N?= 3） and limits of quantitation（LOQs，S/N?= 10） were in the ranges of 0.001－0.17 mg/kg and 0.003－0.55 mg/kg，respectively．The recoveries for the 19 targets at two spiked concentration levels ranged from 65.8% to 97.2%，with relative standard deviations（RSDs，n?= 6） of 4.3%－13%．This method was used for special food safety risk monitoring on the bamboo and wooden products related to food in Guizhou province，and the hidden risks of high pentachlorophenol residues in non-shaped packaging wooden chopping boards were discovered，which could provide an early risk warning for relevant departments． |
| Key Words:wooden chopping board ?sampling in surface ?antiseptic and antifungal agent ?gas chromatography－tandem mass spectrometry（GC－MS/MS） ?risk early warning |
| 引用本文：张权，刘利亚，周贻兵，吴玉田，李磊，林野，郭华，周雪，陈庆园.表层取样法结合气相色谱－串联质谱测定竹木砧板中19种防腐防霉剂残留[J].分析测试学报,2022,41(5):724-730. |
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