干旱区生态环境知识资源中心(Arid): 畜肉中10种镇静剂残留的超高效液相色谱-串联质谱测定方法

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	畜肉中10种镇静剂残留的超高效液相色谱-串联质谱测定方法
其他题名	Determination of Ten Sedative Residues in Livestock Products by Ultra High Performance Liquid Chromatography - Tandem Mass Spectrometry
	张烁 1; 周爽 1; 陈达炜 1; 花镇东 2; 吴永宁 1; 孙承业 3; 赵云峰 1
来源期刊	分析测试学报
ISSN	1004-4957
出版年	2014
卷号	33 期号:11 页码:1213-1218
中文摘要	建立了一种灵敏的超高效液相色谱-串联四极杆质谱(UHPLC-MS/MS)方法,并用于动物肌肉组织(猪肉、牛肉、羊肉)中10种兽药镇静剂的同时测定。样品酶解后,经乙腈提取,MCX固相萃取净化,以ACQUITY UPLC CSH C_(18)色谱柱分离,UPLC - MS/MS的多反应监测(MRM)模式,用同位素稀释内标法(安眠酮采用基质匹配外标法)进行分析。10种镇静剂在0.5~100 mug/L范围内显示良好线性(r~2 ≥0.993 6),其检出限(LOD)不高于0.5 ≥mug/kg,定量下限(LOQ)不高于1.0 mug/kg。在1.0, 5.0,50. 0 mug/kg加标水平下,10种镇静剂的平均回收率为82.0%~116.0%,相对标准偏差(RSDs)为0.6%~12.8%。该方法准确可靠,适用于畜肉中镇静剂多残留的分析。
英文摘要	An ultra high performance liquid chromatography - tandem mass spectrometric (UHPLC - MS/MS) method was established for the determination of 10 sedative (azaperol, azaperone, xylazine, haloperidol, promethazine, acepromazine, propionylpromazine, chloropromazine, methaqualone and diazepam) residues in pork, beef and mutton. After enzymolysis, 10 veterinary drugs were extracted with acetonitrile and cleaned up with an Oasis MCX SPE column. The analysis of the sedatives were achieved on an ACQUITY UPLC CSH C18 column and detected by electrospray ionization - tandem mass spectrometry in the multiple reaction monitoring(MRM) mode. The calibration curves of ten sedatives showed good linearities (r~2≥0. 993 6) in the concentration range of 0. 5 - 100 mug/L. The limits of detection(LODs, S/N≥3) were not more than 0. 5 mug/kg, and the limits of quantitation (LOQs, S/N≥10) were not more than 1. 0 mug/kg. The average recoveries of ten sedatives ranged from 82. 0% to 116. 0% with relative standard deviations (RSDs) of 0. 6% - 12. 8% at the spiked levels of 1. 0,5. 0,50. 0 mug/kg. The results showed that the method was sensitive, and accurate, and was suitable for the determination of sedative residues in animal originated food.
中文关键词	畜肉 ; 兽药 ; 镇静剂 ; 残留 ; 超高效液相色谱-串联质谱
英文关键词	livestock product veterinary drug sedative residue ultra high performance liquid chromatography - tandem mass spectrometry(UHPLC - MS/MS)
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL
WOS研究方向	Chemistry
CSCD记录号	CSCD:5291279
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/231036
作者单位	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, 中国; 2.公安部禁毒情报技术中心, 北京 100193, 中国; 3.中国疾病预防控制中心职业卫生与中毒控制所, 北京 100050, 中国
推荐引用方式 GB/T 7714	张烁,周爽,陈达炜,等. 畜肉中10种镇静剂残留的超高效液相色谱-串联质谱测定方法[J],2014,33(11):1213-1218.
APA	张烁.,周爽.,陈达炜.,花镇东.,吴永宁.,...&赵云峰.(2014).畜肉中10种镇静剂残留的超高效液相色谱-串联质谱测定方法.分析测试学报,33(11),1213-1218.
MLA	张烁,et al."畜肉中10种镇静剂残留的超高效液相色谱-串联质谱测定方法".分析测试学报 33.11(2014):1213-1218.