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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。
An analytical method for the rapid determination of chloramphenicol (CAP) in Holothuria by using isotope dilution-liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) was established. Ammonia was added to the sample, which was extracted with ethyl acetate. After concentration, n-hexane was degreased and purified. The separation was performed on a C18 reversed-phase column with gradient elution with water-acetonitrile as the mobile phase. Multiple reactive ion (MRM) monitoring was performed on a triple quadrupole mass spectrometer equipped with an electrospray ionization source and quantified by isotope dilution internal standard method. The linearity of CAP in the range of 0.1 ~ 2.0μg / L was good, the correlation coefficient was not less than 0.999 3, and the limit of detection (LOD) was 0.06μg / kg with 3 times the signal to noise ratio (S / N) The noise ratio was determined to have a limit of quantitation (LOQ) of 0.1 μg / kg. The recoveries of CAP in sea cucumber were 88.2% ~ 98.2% within 0.1 ~ 3.0μg / kg spike calibration range, and the relative standard deviation (Intra-RSD) was 2.3% ~ 4.1% ) Was 3.6% ~ 4.6%. The method has high sensitivity, easy operation and good stability, and is suitable for qualitative and quantitative detection of chloramphenicol residues in sea cucumber.