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HS/GC-MS/MS法检测海产品中二甲苯
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作者单位
周秀锦,杨会成,邵宏宏,张静,相兴伟,韩超,郑斌 1.舟山出入境检验检疫局2.浙江海洋开发研究院
3.温州出入境检验检疫局
 
基金项目:国家科技支撑计划项目(2012BAD29B06);舟山市社会公益科技计划项目(2015C31049)
中文摘要:建立了顶空进样/气相色谱-串联三重四极杆质谱(HS/GC-MS/MS)检测海产品中3种二甲苯同分异构体的方法。海产品经90 ℃温育和振荡平衡40 min顶空进样,HP-INNOWax色谱柱分离,程序升温,在多反应监测(MRM)模式下进行GC-MS/MS检测,外标法定量。结果表明,3种二甲苯同分异构体在50~1000 μg/kg范围内呈良好线性,相关系数均在099以上,方法检出限为25 μg/kg,定量下限为50 μg/kg。黄鱼样品在60、150、500 μg/kg加标水平下的平均回收率为896%~1124%,相对标准偏差(RSD)不大于115%。采用建立的方法测定了不同海产品中二甲苯同分异构体的含量。该法操作简单、定性准确、灵敏度较高,适于海产品中二甲苯残留量的测定。
中文关键词:顶空进样  气相色谱-串联质谱(GC-MS/MS)  二甲苯  同分异构体  海产品
 
Determination of Three Xylene Isomers in Seafoods by GC-MS/MS Method with Headspace Injection
Abstract:A method based on gas chromatography-triple quadrupole mass spectrometry with headspace(HS/GC-MS/MS) was developed for the determination of three xylene isomers in seafoods.The samples were incubated at 90 ℃ and oscillated for 40 min,then separated on an HP-INNOWax column.The determination of the target compounds were performed by GC-MS/MS under the multiple reaction monitoring(MRM) mode,and the quantification was carried out using the external standard method.The calibration curves for three xylene isomers were linear in the range of 50-1000 μg/kg with their correlation coefficients(r2) larger than 099.The limits of detection(LOD) and quantitation(LOQ) of the method were 25 μg/kg and 50 μg/kg,respectively.The recoveries at three spiked level of 60,150,500 μg/kg were in the range of 896%-1124% with relative standard deviations(RSD) not more than 115%.The method was successfully applied in the determination of xylene isomers in seafoods.With the advantages of simple operation,accuracy and high sensitivity,the method was suitable for the determination of xylene residues in seafoods.
Key Words:headspace  gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)  xylene  isomer  seafood
引用本文:周秀锦,杨会成,邵宏宏,张静,相兴伟,韩超,郑斌.HS/GC-MS/MS法检测海产品中二甲苯[J].分析测试学报,2018,37(7):844-848.
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