UPLC-MS/MS测定羊奶中氯霉素、甲砜霉素、氟苯尼考

Determination of Chlorampheincol, Thiamphenicol and Florfenicol Residues in Sheep Milk by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立液相色谱-串联质谱法测定羊奶中氯霉素、甲砜霉素、氟苯尼考(氟甲砜霉素)残留量的分析方法。样品经乙酸乙酯提取,氮吹浓缩,以乙腈水作为流动相,通过高效液相色谱,采用负离子模式多反应监测,氯霉素用同位素内标定量,甲砜霉素、氟甲砜霉素用外标法定量。氯霉素、甲砜霉素和氟甲砜霉素线性关系良好,其线性方程分别为Y=1.063X+0.006, Y=13.999X+3.861, Y=98.439X-9.476,相关系数R2均大于0.995;氯霉素、甲砜霉素、氟甲砜霉素的定量限为0.089 7, 0.092 5和0.083 6μg/kg;当加标水平在0.1~5.0μg/kg时,回收率在88.8%~112.8%之间,方法的精密度相对标准偏差在0.2%~12.3%之间。该方法简单易行,回收率好,灵敏度高,特异性强,能满足目前大多数羊奶的日常监管检测。

A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) analysis method was established for simultaneous determination of chlorampheincol, thiamphenicol and florfenicol in sheep milk. The sample was extracted with ethyl acetate and concentrated with nitrogen. Mobile phase was acetonitrile and water. The identification and quantification of chloramphenicols residues were carried out by MS/MS in negative eletrospray ionization and multiple reaction monitoring mode. Isotope was used by internal standard quantitation of chlorampheincol, and thiamphenicol and florfenicol were used by external standard method for quantitation. The calibration curves of mixed standard solution showed good linearities with the correlation coefficients(R2) more than 0.995. The linear equations of CAP, TAP and FF were Y=1.063X+0.006, Y=13.999X+3.861 and Y=98.439X-9.476, respectively. The quantification limits were 0.089 7, 0.092 5 and 0.083 6 μg/kg. The average recoveries for the analysis of sheep milk spiked at the range of 0.1-5.0 μg/kg were in the range of 88.8%-112.8%. The relative deviation of within-day precision was 0.2%-12.3%. The proposed method was simple, effective and sensitive, which could meet the needs of daily detection and supervision.