QuEChERS-超高效液相色谱-串联质谱法测定动物源食品中痕量五氯酚及其钠盐

doi:10.3724/SP.J.1123.2018.03017

色谱 ›› 2018, Vol. 36 ›› Issue (6): 518-522.DOI: 10.3724/SP.J.1123.2018.03017

• 生物基质农兽药残留检测专栏 • 上一篇下一篇

QuEChERS-超高效液相色谱-串联质谱法测定动物源食品中痕量五氯酚及其钠盐

王连珠¹, 方恩华², 王彩娟¹, 陈泳¹, 林子旭¹, 徐敦明²

1. 漳州出入境检验检疫局, 福建漳州 363100;
2. 厦门出入境检验检疫局, 福建厦门 361012

收稿日期:2018-03-16 出版日期:2018-06-08 发布日期:2014-04-24
通讯作者: 王连珠,Tel:(0596)2175990,E-mail:3125325899@qq.com
基金资助:
福建省自然科学基金项目（2011J01386，2016J01070）.

Determination of trace pentachlorophenol and its sodium salt in animal-origin foods by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

WANG Lianzhu¹, FANG Enhua², WANG Caijuan¹, CHEN Yong¹, LIN Zixu¹, XU Dunming²

1. Zhangzhou Entry-Exit Inspection and Quarantine Bureau, Zhangzhou 363100, China;
2. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, China

Received:2018-03-16 Online:2018-06-08 Published:2014-04-24
Supported by:
Natural Science Foundation of Fujian Province (Nos.2011J01386,2016J01070).

摘要/Abstract

摘要：

采用改良的QuEChERS-超高效液相色谱-串联质谱（UPLC-MS/MS）技术，建立了动物源食品中痕量五氯酚及其钠盐的测定方法。样品中五氯酚钠在酸性条件下转化为五氯酚，采用1%（v/v）乙酸乙腈超声提取2次，提取液浓缩后分散固相萃取净化，以回收率及基质效应为考察指标，对吸附剂进行了优化。采用Waters Acquity UPLC HSS T3色谱柱梯度洗脱分离，在电喷雾电离（ESI）源、负离子模式和多反应监测模式下检测，基质匹配外标法定量。在1.0、2.0、10.0 μg/kg添加水平下6种基质（猪肉、猪肝、鸡肉、鱼肉、牛奶、鸡蛋）中五氯酚的加标回收率为73.2%~108.4%，相对标准偏差为4.0%~14.8%；定量限（S/N>10）为1.0 μg/kg。该方法简便、灵敏、准确、环保，适用于动物源食品中痕量五氯酚及其钠盐残留的定性定量分析。

关键词: QuEChERS, 超高效液相色谱-串联质谱, 动物源食品, 五氯酚, 五氯酚钠

Abstract:

A method was developed for the determination of trace pentachlorophenol and its sodium salt in animal-origin foods by modified QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Sodium pentachlorophenolate in samples was converted to pentachlorophenol under acidic condition. The pentachlorophenol was extracted twice with acetonitrile containing 1% (v/v) acetic acid by ultrasonic extraction. The extracts were purified by dispersive solid-phase extraction. The usages of dispersive sorbents were optimized based on the recoveries and matrix effects. Chromatographic analysis was conducted on a Waters Acquity UPLC HSS T3 column with gradient elution. The pentachlorophenol was further analyzed by negative electrospray ionization under the multiple reaction monitoring mode. The recoveries at fortification levels of 1.0, 2.0 and 10.0 μg/kg in six matrices (pork, pork liver, chicken, fish, milk and egg) ranged from 73.2% to 108.4% with the relative standard deviations of 4.0%-14.8%. The limits of quantification (S/N>10) were 1.0 μg/kg. The method is simple, sensitive, accurate, economical and environmentally safe, and is suitable for the determination of the trace pentachlorophenol and its sodium salt in animal-origin foods.

Key words: animal-origin foods, pentachlorophenol, QuEChERS, sodium pentachlorophenolate, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号:

O658

王连珠, 方恩华, 王彩娟, 陈泳, 林子旭, 徐敦明. QuEChERS-超高效液相色谱-串联质谱法测定动物源食品中痕量五氯酚及其钠盐[J]. 色谱, 2018, 36(6): 518-522.

WANG Lianzhu, FANG Enhua, WANG Caijuan, CHEN Yong, LIN Zixu, XU Dunming. Determination of trace pentachlorophenol and its sodium salt in animal-origin foods by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(6): 518-522.

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QuEChERS-超高效液相色谱-串联质谱法测定动物源食品中痕量五氯酚及其钠盐

Determination of trace pentachlorophenol and its sodium salt in animal-origin foods by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

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