摘要
建立了利用同位素稀释-液相色谱串联质谱（HPLC-MS/MS）快速检测海参（Holothuria）中氯霉素（chloramphenicol,CAP）残留量的分析方法。样品中加入氨水后,用乙酸乙酯提取,经浓缩后,正己烷去脂净化。采用C18反相色谱柱进行分离,以水-乙腈作为流动相进行梯度洗脱,用配有电喷雾离子源的三重四级杆质谱进行多反应离子（MRM）监测,同位素稀释内标法定量。CAP在0.1~2.0μg/L范围内线性关系良好,相关系数不低于0.999 3,以3倍信噪比（S/N）确定检出限（LOD）为0.06μg/kg,以10倍信噪比确定其定量限（LOQ）为0.1μg/kg。海参中CAP在0.1~3.0μg/kg加标范围内的回收率为88.2%~98.2%,批内相对标准偏差（Intra-RSD）为2.3%~4.1%,批间相对标准偏差（Inter-RSD）为3.6%~4.6%。该方法灵敏度高,操作简便,稳定性好,适用于海参中氯霉素残留量的定性和定量检测。
A method for the rapid determination of chloramphenicol（ CAP） residues in sea cucumber was developed by isotope dilution liquid chromatography- tandem mass spectrometry. The sample,after addition of aqueous ammonia, was extracted with ethyl acetate. The solution was defatted and purified with n- hexane and high speed centrifuga- tion. The targeted compounds were separated on C 18 column（ 150 mm × 2. 1 mm,5μm） using water- acetonitrile as mobile phase by gradient elution,and analyzed by a triple quadruple tandem mass spectrometer with electrospray ioni- zation source（ ESI） and multiple reaction monitoring（ MRM）. The samples were quantified by the internal standards labeled with stable isotopes. The standard curves were linear in the ranges of 0. 1- 5. 0 mg / L for CAP with correlation coefficients（ r2） being more than 0. 999 2. The limits of detection were 0. 06 μg/kg,and the limits of determination were 0. 1 μg / kg. The recoveries of CAP in sea cucumber sample at the fortified levels of 0. 1- 3. 0 μg / kg were in the range of 88. 2%- 98. 2%. The intra- assay and inter- assay RSDs for CAP were in the range of 2. 3%- 4. 1% and 3. 6%- 4. 6%,respectively. The results showed that the method was simple,sensitive and accurate,and suitable for the qualitative and quantitative determination of CAP residues in sea cucumber sample.
出处
《中国渔业质量与标准》
2013年第4期36-41,共6页
Chinese Fishery Quality and Standards
关键词
同位素稀释
液相色谱串联质谱法
海参
氯霉素
残留量
isotope dilution
chloramphenicol（CAP）
liquid chromatography-tandem mass spectrometry
sea cucum-ber
residue
