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当前位置: 首页 > 文章 > 超高效液相色谱-串联质谱法测定液态乳中的壬基酚 乳业科学与技术 2018 (4)
Position: Home > Articles > 超高效液相色谱-串联质谱法测定液态乳中的壬基酚 Journal of Dairy Science and Technology 2018 (4)

超高效液相色谱-串联质谱法测定液态乳中的壬基酚

作  者：
白艳梅;张立佳;李翠枝;吕志勇;高玉杰;谢瑞龙;段建华;胡雪
关键词：
超高效液相色谱-串联质谱;液态乳;玻璃固相萃取小柱;壬基酚
摘  要：
利用超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLCMS/MS)技术建立液态乳中壬基酚(nonylphenol,NP)的检测方法.使用乙腈作为提取溶剂,加饱和氯化钠溶液使乙腈和水分层,采用ProElut PAEs Glass玻璃固相萃取小柱净化,Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm*50 mm,1.7μm)分离,以0.1%氨水-甲醇流动相体系进行梯度洗脱,内标法定量,采用电喷雾离子源(负离子模式),在多反应监测模式下进行测定.结果表明:在1200 ng/mL线性范围内,NP的线性关系良好(R2>0.990),方法的检出限(RS/N=3)为2.0μg/kg,定量限(RS/N=10)为5.0μg/kg;在不同加标量下,方法回收率为74.8%111.5%,相对标准偏差为3.3%9.0%.该方法测定结果准确、本底干扰小、操作简便、重复性好,适用于液态乳中NP的检测.
作  者：
BAI Yanmei;ZHANG Lijia;LI Cuizhi;Lü Zhiyong;GAO Yujie;XIE Ruilong;DUAN Jianhua;HU Xue;Inner Mongolia Yili Industrial Group Co.Ltd.;
单  位：
BAI Yanmei%ZHANG Lijia%LI Cuizhi%Lü Zhiyong%GAO Yujie%XIE Ruilong%DUAN Jianhua%HU Xue%Inner Mongolia Yili Industrial Group Co.Ltd.
关键词：
ultra performance liquid chromatography-tandem mass spectrometry;;liquid milk;;glass solid phase extraction catridge;;nonylphenol
摘  要：
A method for the determination of nonylphenol in liquid milk by using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed. Samples were extracted using acetonitrile as extraction solvent and the organic phase was separated from the aqueous phase by adding saturated sodium chloride solution. The analyte was cleaned up using a Pro Elut PAEs Glass solid-phase extraction catridge and then separated on a Waters ACQUITY UPLC BEH C18 column(2.1 mm × 50 mm, 1.7 μm) using gradient elution with 0.1% ammonia watermethanol as mobile phase. The detection was performed by negative electrospray ionization under the multiple reaction monitoring mode and the quantitation was carried out by an internal standard method. The results showed a good linear relationship(R~2 > 0.990) in then range from 1 to 200 ng/mL. The limit of detection(LOD, R_(S/N) = 3)was 2.0 μg/kg and the limit of quantitation(LOQ, RS/N = 10)was 5 μg/kg. The recovery rate of the method for spiked samples was between 74.8% and 111.5% with relative standard deviation of 3.3%-9.0%. In general, the method was accurate, simple and reproducible and exhibited low background inference and it was thus suitable for the analysis of nonylphenol in liquid milk.

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