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气相色谱-串联质谱法测定植物源驱蚊产品中82种风险性化学物质
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李红艳,刘英,李长于,王瑾 1. 浙江省产品质量安全科学研究院浙江 杭州 310018 2. 杭州职业技术学院 生态健康学院 浙江 杭州 310018 3. 浙江方圆检测集团股份有限公司浙江 杭州 310018 
基金项目:浙江省市场监管管理局科技计划项目(20210102);浙江省市场监管雏鹰计划重大培育项目(CY202109)
中文摘要:为同时筛查植物源驱蚊产品中致敏性芳香剂和农药化合物,建立了一种基于溶剂提取/气相色谱-串联质谱(GC-MS/MS)同时检测78种致敏性芳香剂和4种农药化合物的方法。采用极性色谱柱Agilent VF-WAXms进行色谱分离,通过不同的特征离子对对部分共流出化合物进行定性定量分析。以阳性样品为研究对象对提取溶剂和提取时间进行优化,确定最佳提取条件为:以二氯甲烷为提取溶剂,在30 ℃恒温条件下超声提取30 min。结果表明,82种目标化合物在对应质量浓度范围内具有良好的线性关系,相关系数(r)均大于0.992 0,定量下限为0.02 ~ 5.0 mg/kg,回收率为60.0% ~ 120%,相对标准偏差(RSD)不大于9.5%。将该方法用于驱蚊贴、驱蚊扣、驱蚊液和驱蚊凝胶等29个样品的筛查,共检出33种致敏性芳香剂和1种农药(驱蚊酯)。80%以上的样品中检出α-蒎烯、β-蒎烯和D-柠檬烯等11种致敏性芳香剂,最高含量为116 ~ 21 140 mg/kg;3个驱蚊液中检出驱蚊酯,含量为10 200 ~ 21 350 mg/kg。该方法操作简单、结果准确,可用于驱蚊产品中致敏性芳香剂和农药化合物的同时筛查和含量测定。
中文关键词:气相色谱-串联质谱(GC-MS/MS)  驱蚊产品  致敏性芳香剂  农药
 
Determination of 82 Risk Chemicals in Plant Mosquito Repellent Products by Gas Chromatography-Tandem Mass Spectrometry
Abstract:A solvent extraction/gas chromatography-tandem mass spectrometry(GC-MS/MS) was established for the simultaneous detection of 78 allergenic aromatics and 4 pesticide compounds in plant mosquito repellent products.The polar chromatographic column Agilent VF-WAXms was used for chromatographic separation,and some of the co-efflux compounds were analyzed qualitatively and quantitatively by different characteristic ion pairs.The extraction conditions of samples were optimized by using positive samples as the research object.The contents of multiple target substances in the samples were compared under different extraction solvents and different extraction time conditions.The optimal extraction conditions were determined by using dichloromethane as the extraction solvent and ultrasonic extraction at 30 ℃ for 30 min.The results showed that there were good linear relationships for 82 target compounds in the respective concentration ranges,with their correlation coefficients(r) larger than 0.992 0.The limits of quantitation were in the range of 0.02-5.0 mg/kg.The recoveries ranged from 60.0% to 120%,with relative standard deviations(RSDs) not more than 9.5%.The method was used to screen 29 samples including mosquito repellent stickers,mosquito repellent buttons,mosquito repellent liquids and mosquito repellent gels.A total of 33 allergenic aromatics and 1 pesticide(ethyl butylacetylaminopropionate) were detected.11 allergenic aromatics including α-pinene,β-pinene and D-limonene were found in more than 80% of the samples,with a maximum content range of 116-21 140 mg/kg.Meanwhile,ethyl butylacetylaminopropionate was detected in 3 mosquito repellent liquids,with a content range of 10 200-21 350 mg/kg.This method is simple,accurate and reliable,and it could be used for the simultaneous targeted screening and determination on allergenic aromatics and pesticides in mosquito repellent products.
Key Words:gas chromatography-tandem mass spectrometry(GC-MS/MS)  mosquito repellent product  allergenic aromatics  pesticide
引用本文:李红艳,刘英,李长于,王瑾.气相色谱-串联质谱法测定植物源驱蚊产品中82种风险性化学物质[J].分析测试学报,2023,(1):1-10.
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