动物营养学报 >

2018 , Vol. 30 >Issue 10: 4087 - 4094

DOI: https://doi.org/10.3969/j.issn.1006-267x.2018.10.034

实验方法 Experimental Methods

猪肝、牛肉、羊肉中5种β-受体激动剂残留的超高效液相色谱-串联质谱分析方法的建立

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  • 连云港市畜产品质量监督检验测试中心, 连云港 222000
张苏珍(1988-),女,江苏连云港人,硕士研究生,从事畜产品质量安全与检测研究。E-mail:xsdzsz@126.com

收稿日期: 2018-03-20

  网络出版日期: 2018-10-20

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UPLC-MS/MS Method for the Determination of Five β-agonists Residue in Pork Liver, Beef and Mutton

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  • Lianyungang Municipal Quality Supervision and Inspection Center for Animal Products, Lianyungang 222000, China

Received date: 2018-03-20

  Online published: 2018-10-20

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摘要

本试验旨在建立猪肝、牛肉、羊肉中5种β-受体激动剂残留的超高效液相色谱-串联质谱（UPLC-MS/MS）快速检测方法。样品用80%的乙腈提取，经过PRiME HLB固相萃取柱一步净化，氮吹浓缩，最后用10%甲醇复溶。以10 mmol/L乙酸铵水溶液-10 mmol/L乙酸铵甲醇溶液（pH=5）作为流动相进行梯度洗脱，采用多反应监测模式进行测定，内标法定量。5种β-受体激动剂浓度在0.5~50.0 ng/mL呈现良好的线性关系，相关系数（R2）在0.999 63~0.999 96。5种β-受体激动剂浓度为0.5、1.0、5.0 μg/kg时，在猪肝中回收率为93.7%~106.1%，牛肉中回收率为95.2%~104.0%，羊肉中回收率为95.1%~106.0%。通过试验得出该方法具有较好的准确度和重复性。按照特征离子色谱峰信噪比（S/N）=3得出，5种β-受体激动剂检出限为0.01~0.04 μg/kg，定量限为0.02~0.15 μg/kg。本法操作简便，灵敏度高，准确度好，适合大批量畜产品中β-受体激动剂残留的检测分析。

关键词： 超高效液相色谱-串联质谱; β -受体激动剂; 畜产品

本文引用格式

张苏珍, 王益军, 田蕴, 贺燕, 葛敏 . 猪肝、牛肉、羊肉中5种β-受体激动剂残留的超高效液相色谱-串联质谱分析方法的建立[J]. 动物营养学报, 2018 , 30(10) : 4087 -4094 . DOI: 10.3969/j.issn.1006-267x.2018.10.034

Abstract

The aim of this study was to establish a UPLC-MS/MS method for rapid determination of five β-agonists in pork liver, beef and mutton. The five β-agonists in samples were extracted with 80% acetonitrile, purified by PRiME HLB solid phase extraction column, concentrated by nitrogen, and finally dissolved with 10% methanol. A gradient elution was performed using 10 mmol/L ammonium acetate aqueous solution-10 mmol/L ammonium acetate methanol (pH=5) as a mobile phase. The multi-reaction monitoring (MRM) mode was used for the determination, and internal standard method was used for quantification. The concentration of five β-agonists showed good linearity in the range of 0.5 to 50.0 ng/mL with the coefficient correlation (R2) between 0.999 63 to 0.999 96. At the standard addition levels of 0.5, 1.0 and 5.0 μg/kg, the average recovery ratio of five β-agonists was 93.7% to 106.1% in pork liver, 95.2% to 104.0% in beef, and 95.1% to 106.0% in mutton. The test indicated that the method showed good accuracy and repeatability. Based on S/N=3, the detection limit of five β-agonists was 0.01 to 0.04 μg/kg, and quantitation limit was 0.02 to 0.15 μg/kg. This method is simple, sensitive, accurate, and suitable for large quantities animal products detection analysis.

Key words： UPLC-MS/MS; β-agonists; animal products

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