气相色谱-质谱法同时测定动物尿样中莱克多巴胺和克伦特罗  被引量:15

Simultaneous Determination of Ractopamine and Clenbuterol Residues in Animal Urine with Gas Chromatography-Mass Spectrometry

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作  者:应永飞[1] 皮雄娥[2] 吴平谷[3] 陈慧华[1] 朱聪英[1] 陆春波[1] 

机构地区:[1]浙江省畜产品质量安全检测中心,浙江杭州310020 [2]浙江省农业科学院植物保护与微生物所,浙江杭州310021 [3]浙江省疾病预防控制中心,浙江杭州310020

出  处:《质谱学报》2006年第2期74-78,共5页Journal of Chinese Mass Spectrometry Society

基  金:浙江省重点科技攻关项目(No.2005C22029)资助

摘  要:建立了固相萃取-气相色谱-质谱法(SPE-GC/MS)同时测定动物尿样中的莱克多巴胺和克伦特罗的方法。试样中的药物经乙酸乙酯提取后,经SLH固相萃取柱净化,氮吹至干,衍生化后进行气相色谱一质谱测定。两种药物的检出限均为0.3μg/L,定量限均为1.0μg/L,线性范围为0.02~1.0μg/L。加标浓度在4.0~20.0μg/L范围内.莱克多巴胺加标回收率为78.6%~101.2%,批内相对标准偏差≤7.0%;克伦特罗加标回收率为92.3%~112.2%.批内相对标准偏差≤6.9%。A new solid phase extraction-gas chromatography-mass spectrometry (SPE-GC/ MS) method for simultaneous determination of ractopamine and clenbuterol in animal urine was reported. The drugs were extracted with ethyl acetate from sample. The extraction was evaporated at 40℃. After the residue was dissolved in ethyl acetate, it was purified by passing through SLH solid-phase extraction (SPE) cartridges. The eluate was evaporated by nitrogen blow and derivatizated with BSTFA, and then assayed by GC/MS. The limits of detection (LOD) were 0.3μg/L, and the limits of quantitation (LOQ) were 1.0μg/L. The calibration curves were linear between 0. 02 μg/mL and 1.0μg/mL for ractopamine and clenbuterol. Recoveries of ractopamine and clenbuterol were 78. 6%-101. 2%and 92. 3%- 112.2%, and the intra-relative standard deviation (n=5) less than 7.0% and 6.9%, respectively, at spiked levels of 4.0-20μg/L.

关 键 词:固相萃取-气相色谱-质谱法 莱克多巴胺 克伦特罗 残留量 动物尿样 

分 类 号:O657.63[理学—分析化学] R974.3[理学—化学]

 

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