高压液相色谱-质谱联用法测定牙鲆中氯霉素残留量  

The determination of residues of chloramphenicol in paralichthys olivaceus with high press liquid chromatography mass method

作　　者：李兆新[1] 耿霞[1] 刘莹[2] 王慧[2] 王红艳[2] 李平 王志明 

机构地区：[1]中国水产科学研究院黄海水产研究所国家水产品质量监督检验中心,青岛266071 [2]中国海洋大学,青岛266003 [3]安捷伦亚太环境分析实验室,北京100000

出　　处：《海洋水产研究》2005年第5期39-44,共6页Marine Fisheries Research

基　　金：国家科技攻关项目(2002BA906A39)资助

摘　　要：采用高压液相色谱-电喷雾离子阱质谱法(HPLC-MS-Ion Trap)对牙鲆中氯霉素残留量进行了研究。用乙酸乙酯作为提取溶剂,采用液-液萃取法提取样品中氯霉素,经浓缩净化处理后直接进样分析。质谱条件为,碎裂电压115V,锥孔电压25V,二级质谱电压0.9V,智能碎裂模式(SPS)。对氯霉素标准液进行了定性分析,得到氯霉素的一级分子离子峰m/z321和m/z323及二级质谱特征离子峰m/z194、m/z257和m/z176。以m/z257和m/z194的峰面积之和代表氯霉素的质谱峰面积,以此峰面积进行定量计算。在0.1～10μg/kg浓度范围内得到线性方程Y=13180.1X+5048.2,相关系数0.99961;方法的检测限为0.1μg/kg;样品添加回收率98.2%～111.4%,相对标准偏差(n=3)7.8%～10.2%;并测定了8个牙鲆样品,氯霉素残留量为0.99～5.62μg/kg。The residues of chloramphenicol in Paralichthys olivaceus samples are analyzed with HPLC-MS-Ion Trap. Chloramphenicol is extracted by ethyl acetate with a liquid/liquid method. After purification the extracted solution is tested by HPLC-MS directly. The MS working conditions are as follows, fragmentation voltage 115 V, wimble voltage 25 V,the second fragmentation voltage 0.9 V. Chloramphenicol standard solution is qualitatively analyzed. The spectrums of 1st grade mass molecule ions, m/z 321 and m/z 323, are given out. The 2nd grade mass spectrums of molecule ions, m/z 194,m/z 257 and m/z 176 ,are also given out. The total area of rn/z 194 and m/z 257 represents the area of chloramphenicol. This area is used for quantitative analysis. The liner equation is Y= 13 180. 1X＋ 5 048.2 （0.1 - 10 μg/kg）. The correlation coefficient is 0. 999 61. The testing limit is 0.1μg/kg. The recovery is 98.2% 111.4%（1-5μg/kg）. Relative standard deviation is 7.8% -10.2%（n=3）. 8 samples are analyzed using this method. The residues of chloramphenicol are from 0.99μg/kg to 5.62μg/kg.

关 键 词：氯霉素 牙鲆 残留 高压液相色谱 质谱 

分 类 号：O657.72[理学—分析化学] O657.63[理学—化学]