固相萃取-超高效液相色谱-串联质谱法测定畜产品中残留的22种磺胺类药物
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(1.国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京 100021; ;2.浙江省食品药品检验研究院,浙江 杭州 310052;3.岛津企业管理(中国)有限公司,北京 100020)

作者简介:

高洁 女 助理研究员 研究方向为食品安全理化检测E-mail:gaojie@cfsa.net.cn通信作者:赵云峰 男 研究员 研究方向为食品安全理化检测E-mail:zhaoyf@cfsa.net.cn

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基金项目:

国家自然科学基金青年科学基金项目(21607035);国家高技术研究发展计划(863计划)项目(2012AA101603)


Determination of 22 sulfonamides in livestock products by ultra high performance liquid chromatography-tandem mass spectrometry coupled with solid phase extraction
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(1.Key Laboratory of Food Safety Risk Assessment of Ministry of Health, China National Center for Food Safety and Risk Assessment,Beijing 100021, China;2.Zhejiang Institute for Food and Drug Control, Zhejiang Hangzhou 310052, China;3.Shimadzu (China) Co., LTD, Beijing 100020, China)

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    摘要:

    目的 建立畜产品中22种磺胺类药物残留的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。方法 样品经乙腈涡旋提取,正己烷除脂后,阳离子交换固相萃取柱净化,再经Waters Acquity UPLC BEH C18(2.1 mm×100 mm, 1.7 μm)色谱柱分离,在电喷雾正离子多反应监测模式下进行测定。结果 22种磺胺类药物在一定的浓度范围内线性关系良好,相关系数(r)>0.997。在猪肉、猪肝、猪肾3种基质中,22种磺胺类药物的检出限为0.03~0.3 μg/kg,定量限为0.1~1 μg/kg。在1、2、5 μg/kg 三个添加水平下,其加标回收率为63.0%~115.6%,相对标准偏差为1.2%~15.9%。结论 该方法快速、简便、准确可靠,适用于畜产品中22种磺胺类药物的同时检测。

    Abstract:

    Objective To establish a method for the determination of 22 sulfonamides in livestock products by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were extracted by acetonitrile and the fat was removed by hexane. Then the extract was purified by cation exchange solid phase extraction. The analytes were separated on a Waters Acquity UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm) and detected by positive electrospray ionization in multiple reactions monitoring (MRM). Results The method showed a good linearity within a certain concentration ranges with relative coefficient r>0.997. The detection limits of 22 sulfonamides in porcine muscle, liver, and kidney were 0.03-0.3 μg/kg, and the quantification limits were 0.1-1 μg/kg. The average recoveries of 22 sulfonamides at the spiking levels of 1,2 and 5 μg/kg were in the range of 63.0%-115.6%, with the relative standard deviations in the range of 1.2%-15.9%. Conclusion The method was rapid, simple and accurate for the simultaneous determination of 22 sulfonamides in livestock products.

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高洁,陈达炜,丁宇琦,李长坤,赵云峰.固相萃取-超高效液相色谱-串联质谱法测定畜产品中残留的22种磺胺类药物[J].中国食品卫生杂志,2018,30(1):28-34.

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  • 收稿日期:2018-01-16
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  • 在线发布日期: 2018-04-02
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