超声辅助萃取-液相色谱-串联质谱法同时检测水产品中11种有机磷酸酯类阻燃剂

索莉莉; 朱群英; 胡美华

doi:10.13386/j.issn1002-0306.2018.06.038

超声辅助萃取-液相色谱-串联质谱法同时检测水产品中11种有机磷酸酯类阻燃剂

南昌市疾病预防控制中心, 江苏南昌 330038

基金项目:

南昌市科技局指导性科技计划项目(洪科发计字【2014-196】号第14项)。

详细信息

作者简介:
索莉莉(1985-),女,硕士研究生,主管技师,研究方向:食品理化检验,E-mail:slluoii@163.com。

中图分类号: TS254.7
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出版历程
- 收稿日期: 2017-07-16
- 网络出版日期: 2020-11-23
- 刊出日期: 2018-03-14

Simultaneous determination of 11 organophosphate esters in aquatic product by ultrasound-assisted extraction coupled with LC-MS/MS

Nanchang Center for Disease Control and Prevention, Nanchang 330038, China

摘要

摘要: 目的:建立了超声辅助萃取技术结合高效液相色谱-串联质谱联用技术同时提取和测定水产品中11种有机磷酸酯类阻燃剂的分析方法。方法:采用超声辅助技术对样品进行萃取,高效液相色谱-串联质谱联用技术分离检测,正离子多反应监测(MRM)模式定量分析。考察了萃取溶剂、萃取体积、萃取时间和不同流动相对实验结果的影响。结果:二氯甲烷为萃取溶剂,萃取体积为 10 mL,萃取时间为 10 min,0.1%甲酸甲醇-0.1%甲酸水为流动相,以梯度洗脱的方式分离为最优条件。在该条件下,11种有机磷酸酯类阻燃剂分离良好,相关系数大于0.998。加标回收率为91.2%~110.5%,相对标准偏差为0.14%~6.6%。方法定量限为0.020~5.71 μg·kg^-1。结论:该方法前处理简单、快速、萃取效率高,能够应用于水产品中11种有机磷酸酯类阻燃剂的分析检测。
- 超声辅助萃取 /
- 液相色谱-串联质谱 /
- 水产品 /
- 有机磷酸酯类阻燃剂
Abstract: Objective:An effective method was developed for the simultaneous determination of 11 organophosphate esters in aquatic product,based on ultrasound-assisted extraction coupled with LC-MS/MS. Methods:Samples were extracted by ultrasonic,and then the target compounds were analyzed by LC-MS/MS under positive electrospray ionization,and quantified by the multiple reaction monitoring. The conditions,including extraction solvent,extraction volume,extraction time and moving phase,were studied. Result:Under the optimal experimental conditions,dichloromethane was used as the extraction solvent with extraction volume 10 mL,ultrasonic time was 10 min,and mobile phase was methanol containing 0.1% formic acid-water containing 0.1% formic acid. 11 kinds of organophosphate esters were successfully separated,the correlation coefficients were more than 0.998,the quantitation limits ranged from 0.020~5.71 μg·kg^-1,the recoveries were in the range of 91.2%~110.5% with the RSDs of 0.14%~6.6%. Conclusion:The method pretreatment was simple,rapid and effective,and could be applied in the determination of 11 kinds of organophosphate esters in aquatic product.
- ultrasound-assisted extraction /
- LC-MS/MS /
- aquatic product /
- organophosphate esters

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参考文献(1)

[1]	Analysis and Determination

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