超高效液相色谱-三重四级杆串联质谱法同时测定饮料中11种磷酸酯类增塑剂含量
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(1.中国检验检疫科学研究院,北京 100176;2.中国医科大学,辽宁 沈阳 110122)

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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:┣┣(中)通信作者┫┫张峰 男 研究员 研究方向为分析化学E-mail:fengzhang@126.com

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国家重点研发计划课题(2017YFC1601305)


Simultaneous determination of organophosphate eater plasticizers used in beverage by ultra high performance liquid chromatography-triple duadrupole tandem mass spectrometry
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(1.Chinese Academy of Inspection and Quarantine, Beijing 100176, China;2.China Medical University, Liaoning Shenyang 110122, China)

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    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,2.5 μm)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2.5~50 μg/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。

    Abstract:

    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 C18 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.

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凌云,雍炜,何佩霞,毕静波,姚美伊,姚桂红,张峰.超高效液相色谱-三重四级杆串联质谱法同时测定饮料中11种磷酸酯类增塑剂含量[J].中国食品卫生杂志,2019,31(6):528-532.

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  • 收稿日期:2019-09-12
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  • 在线发布日期: 2020-01-14
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