A method for the determination of matrine and rotenone residues in aquatic products by liquid chromatography-electrospray tandem mass spectrometric method was described. The analytes were extracted from homogenised tissue using acetonitrile-ammonium acetate buffer. After adding sodium chloride to separate to the analytes by salting-out, the n-hexane was used to defat. Rapid chromatographic separation was achieved on Agilent Zobax SB-C18 column in the mobile phase composition of 20 mmol/L ammonium acetate buffer consisting formic acid as ion-pair agent and acetonitrile. Detection is carried out using poistive-ion electrospray tandem mass spectrometry. The method is accurate, specific and sensitive for the determination of matrine and rotenone residues in aquatic products in the concentration range of 0. 001- 0. 05 mg/kg. The average recoveries and the relative standard deviation ranged from 82.3％-96.1％ and 6.1％- 12.6％, respectively, in spiked tissue samples at concentration levels ranging from 0. 002 mg/kg to 0.2 mg/kg of each analytes. The limits of detection (LOD) of matrine and rotenone were 0.86 and 0.53 μg/kg respectively. This method is suitable for the determination of matrine and rotenone residues in aquactic products and the pharmacokinetics study.%建立了液相色谱-串联质谱同时检测水产品中苦参碱与鱼藤酮残留的方法.试样以乙酸铵缓冲液乙腈提取,提取液中加入 NaCl盐析后,以正己烷除脂净化.采用 Agilent Zobax SB-C<,18>色谱柱,以乙酸铵缓冲液-乙腈为流动相,梯度洗脱分离后,采用电喷雾电离源串联质谱的正离子模式测定.分析物在0.001～0.05mg/kg范围内线性关系良好,线性相关系数大于0.99.在0.002～0.2 mg/kg浓度范围内,平均加标回收率为82.3%～96.1%;相对标准偏差为6.1%～12.6%.苦参碱和鱼藤酮的检出限分别为0.86和0.53 ug/kg.本方法可靠、稳定,满足水产品中苦参碱和鱼藤酮残留检测以及药代动力学研究的需要.
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