超高效液相色谱串联质谱法测定猪尿中22种β_2-受体激动剂残留量  

Determination residues of 22 β_2-agonist in pig urine by ultra high performance liquid chromatography tandem mass spectrometry

作　　者：郭平[1,2] 万建春[2] 祝建新[2] 占春瑞[2] 石磊[2] 丁双阳[1] 

机构地区：[1]中国农业大学动物医学院,北京100193 [2]江西出入境检验检疫局检验检疫综合技术中心,南昌330038

出　　处：《分析试验室》2017年第6期717-721,共5页Chinese Journal of Analysis Laboratory

摘　　要：建立了猪尿中22种β2-受体激动剂残留量超高效液相色谱串联质谱的测定方法。样品加入0.2 mol/L乙酸铵缓冲溶液和β-葡萄糖醛苷酶/芳基硫酸酯酶,在55℃酶解4 h后加入三氯乙酸调节pH,阳离子交换固相萃取小柱净化,依次用2%乙酸、甲醇、正己烷、甲醇、0.5%氨水溶液、甲醇淋洗,5%氨化甲醇洗脱,洗脱液在40℃下氮吹至干,用0.5 mL甲醇-0.1%甲酸溶液(V/V=1:9)溶解样品。22种β2-受体激动剂检出限在0.03~0.3μg/kg之间,加标回收率在70.1%~120.0%之间,相对标准偏差在0.87%~16%范围内。改进了β2-受体激动剂残留量检测前处理的酶解方法和固相萃取净化技术,方法的灵敏度高,也提高了方法的检测效率。A method for the determination of 22 β2-agonist residues in the pig urine by ultra high performance liquid chromatography tandem mass spectrometry was developed. After the sample preparation, the sample was diluted with 0. 2 mol/L ammonium acetate buffer solution and mixed with β-glucoronidase/arylsulfatase for enzymatic hydrolysis at 55℃ for 4 h. After adjusting the pH of the solution with triehloroaeetic acid, the sample was purified by cation exchange solid phase extraction column. After the column was raised cleaned with 2% acetic acid, methanol, n-hexane, methanol, 0. 5% ammonia and methanol, all analytes were eluted by 5% ammoniated methanol. The eluent was evaporated at 40℃ to dryness under a gentle stream of nitrogen, and redissolved with 0. 5 mL methanol-0. 1% formic acid solution （V： V = 1：9）. The detection limits of 22 β2-agonist were between 0. 03 μg/kg and 0. 3μg/kg. The recoveries of methods were between 70. 1% and 120. 0% , with the relative standard deviations of 0. 87% - 16%. This method has been improved in enzymatic hydrolysis and solid phase extraction technology. Due to the high sensitivity, this method has also improved the detection efficiency.

关 键 词：猪尿 β2-受激动剂 快速酶解 超高效液相色谱串联质谱法 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]