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猪肉中92种兽药残留的UPLC-Qtrap高通量筛查和定量方法的研究
孙雷
0
(中国兽医药品监察所)
摘要:
结合简单快速的前处理方法和超高压液相色谱-三重四级杆/线性离子阱串联质谱(UPLC-Qtrap)技术,建立了猪肉中92种兽药残留同时检测的高通量筛查和定量方法。样品经简单快速的前处理后,经Kinetex Core-Shell色谱柱分离,分析时间仅13.5 分钟。质谱采用多反应监测-信息关联-增强子离子(MRM-IDA-EPI)采集方式及谱库检索技术,通过化合物的保留时间、离子对丰度比以及EPI标准谱库检索对比,可完成对92种兽药的快速筛查和确证。采用基质匹配标准溶液外标法定量。结果表明:在1~50 ng/mL猪肉基质匹配标准溶液浓度范围内呈良好线性关系,相关系数R2均大于0.990;方法定量限均为1 ng/g;在1~10 ng/g的添加浓度范围内92种药物的回收率为50%~120%,批内批间相对标准偏差均小于20%。
关键词:  猪肉  兽药残留  UPLC-Qtrap  筛查和定量
DOI:
投稿时间:2017-04-10修订日期:2017-05-24
基金项目:
The Study on High-throughput Screening and Quantitative Method for 92 Veterinary Drugs Residues in Pig Muscle by UPLC-Qtrap
(China Institute of Veterinary Drug Control)
Abstract:
A high-throughput screening and quantitative method by UPLC-QTRAP was established for the determination of 92 veterinary drugs residues in pig muscle. The sample preparation is simple and rapid. The separation of 92 veterinary drugs is performed on the column of kinetex core-shell and total run time is 13.5 min. The data is acquired by multiple reactions monitoring with information-dependent acquisition of enhanced product ion (MRM-IDA-EPI) mode followed with database searching. The veterinary drugs are screened and confirmed by retention times, ion ratio and the database searching by EPI library. The method is quantified by matrix matched-standard solution curves. The calibration curves were good linear between the peak areas and the concentrations of 2~50ng/mL with the correlation coefficient R2>0.990. The limit of detection of 92 veterinary drugs is 1 ng/g. The average recoveries from spiked pig muscle at the concentrations of 1~10 ng/g ranged 50%~120%. The intra- and inter-batch variation coefficients are both less than 20%.
Key words:  pig muscle  veterinary drug residues  UPLC-Qtrap  screening and quantitative method

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