摘要
目的建立超高效液相色谱-三重四级杆串联质谱(UPLC-MS/MS)同时测定饮料中11种磷酸酯类增塑剂含量的检测方法。方法饮料样品用乙腈液液萃取,采用N-丙基乙二胺(PSA)进行固相基质分散净化,C18色谱柱(2.1 mm×100 mm,2.5μm)分离,0.1%甲酸水溶液和甲醇为流动相进行梯度洗脱,采用电喷雾离子源,正离子模式进行多反应监测。结果 11种目标物的定量限在2.5~50μg/L之间,加标浓度范围下,平均回收率在82.4%~113.0%之间,相对标准偏差(RSD)在3.8%~17.6%之间。结论该方法简单快速,灵敏度高,准确度高,可用于饮料中磷酸酯类增塑剂的风险监测。
Objective A method was developed for the simultaneous determination of 11 organophosphate ester plasticizers in beverage by ultra high performance liquid chromatography-triple duadrupole tandem mass spectrometry(UPLC-MS/MS). Methods The sample was liquid-liquid extracted with acetonitrile, and purified by matrix solid dispersion using primary secondary amine(PSA). The compounds were separated on a C18 chromatographic column(2.1 mm×100 mm,2.5 μm)with the gradient elution of 0.1% formic acid aqueous solution and methanol as mobile phase. The analytes were detected by electrospray ionization source in the positive ion mode and multiple reactions monitoring mode. Results The result showed that the limits of quantification were in the range of 2.5-50 μg/L, the average spiked recoveries were in the range of 82.4%-113.0%, and the relative standard deviations(RSD) were in the range of 3.8%-17.6%. Conclusion This method was simple, rapid, sensitive, accurate, and could be used for the monitoring and supervision of organophosphates in beverage.
作者
凌云
雍炜
何佩霞
毕静波
姚美伊
姚桂红
张峰
LING Yun;YONG Wei;HE Peixia;BI Jingbo;YAO Meiyi;YAO Guihong;ZHANG Feng(Chinese Academy of Inspection and Quarantine,Beijing 100176,China;China Medical University,Liaoning Shenyang 110122,China)
出处
《中国食品卫生杂志》
CSCD
北大核心
2019年第6期528-532,共5页
Chinese Journal of Food Hygiene
基金
国家重点研发计划课题(2017YFC1601305)
关键词
超高效液相色谱-三重四级杆串联质谱
磷酸酯
增塑剂
饮料
Ultra high performance liquid chromatography-triple duadrupole tandem mass spectrometry
organo-phosphate
plasticizer
beverage
作者简介
凌云,女,研究员,研究方向为营养与食品卫生学,E-mail:lingyun_505@163.com;通信作者:张峰,男,研究员,研究方向为分析化学,E-mail:fengzhang@126.com。
