三重四极杆气质联用法测定熟肉及其制品中多组分β-受体激动剂残留量
Determination of muti-component beta-agonist residues in meat and its products by triple quadrupole gas chromatography-mass spectrometry
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摘要: 通过未检出β-受体激动剂的熟肉作为空白样品,采用酶解法将动物组织彻底分解,以固相萃取小柱进行萃取净化,净化液经衍生剂后经毛细管色谱柱程序升温分离,利用GC-MS/MS多反应监测模式(MRM模式)对目标物进行采集,以氘代同位素化合物为内标进行内标法定量.采用质控样品和加标回收率评价方法的准确度,以回收率的相对标准偏差(RSD)评价方法的精密度.12种β-受体激动剂在0.20-50 μg·kg-1范围线性关系良好,相关系数在0.9925-0.9995范围内,检出限为0.2-0.4 μg·kg-1.空白样品在1.00、10.0、50.0 μg·kg-1水平的回收率为65.5%-110.7%;RSD为1.16%-8.93%.此方法假阳性率低、准确、可靠.
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关键词:
- 三重四极杆气质联用法 /
- 多组分 /
- β-受体激动剂 /
- 熟肉及其制品
Abstract: Using meat without beta-agonist residues as the blank sample, then enzyme was used to let the animal tissues thoroughly decomposed, and the solid phase extraction was used to cleanse the sample. After extraction and purification, the purified liquid was separated by temperature programmed capillary column after derivatives. The multi-reaction monitoring mode (MRM model) of GC_MS/MS was used for date acquisition, and quantified by internal standard method with deuterium isotope compound as internal standard. Accuracy of the method was based on quality control samples and standard addition recovery rate.The relative standard deviation (RSD) of recovery rate was used to evaluate the accuracy of the method. The correlation coefficient of the 12 beta-agonist residues was in the range of 0.9925-0.9995, and the detection limit was 0.2-0.4 μg·kg-1. The recovery o was 65.5%-110.7% and RSD was 1.16%-8.93%. This method was accurate, reliable and has low false positive rate.-
Key words:
- GC-MS/MS /
- muti-component /
- beta-agonist rediues /
- meat and its products
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