QuEChERS-UPLC-MS/MS测定宣威火腿中氯霉素残留量

Determination of Chloramphenicol Residue in Xuanwei Ham by Quechers-UPLC-MS/MS

建立以Bond Elut QuEChERS EMR-Lipid为前处理测定云南宣威火腿中氯霉素残留检测的超高效液相色谱-串联质谱的方法。采用QuEChERS流程,样品经5%甲酸乙腈提取,经EMR-Lipid增强型脂质去除净化管和EMR-Lipid Polish反萃管进一步净化,取乙腈层氮吹浓缩至近干,加入1.00 mL初始流动相复溶,过0.2μm微孔滤膜。用超纯水-甲醇作流动相,比例为55∶45 (V/V)等梯度洗脱,经Agilent Eclipse-plus C_(18)色谱柱分离,采用电子喷雾离子源ESI-和多反应监测MRM模式测定。流动相配制标准曲线,内标法定量。氯霉素在0.5~50 ng/mL测定范围呈良好线性关系,相关系数R^(2)大于0.999,方法检出限为0.06μg/kg,定量限为0.18μg/kg,在1.0, 5.0和10.0μg/kg 3个水平的加标回收率为79.4%~108.7%,相对标准偏差S_(RSD)为1.97%~5.85%(n=6)。该方法简便、快速、可靠,可用于宣威火腿中氯霉素的检测分析。

To establish the determination of chloramphenicol residues in Xuanwei ham using Bond Elut QuEChERS EMR-lipid as pre-treatment by UPLC-MS/MS, using the QuEChERS process, the samples were extracted by 5% formic acid acetonitrile, and purified by EMR-lipid enhanced Lipid tube and EMR-lipid Polish reverse extraction tube. The acetonitrile layer was condensed by nitrogen blowing until nearly dry, then redissolved by adding 1.00 mL initial mobile phase, and passed through 0.2 μm microporous membrane. Ultra-pure water and methanol were used as mobile phase with a ratio of 55∶45(V/V). The separation was used by Agilent Eclipse-Plus C_(18) column and determined by ESI-and MRM mode. Standard solution was prepared by mobile phase and internal standard quantitative method. The result had good linear relationships in the range of 0.5-50 ng/mL. The correlation coefficient R^(2) was greater than 0.999. The limit of detection was 0.06 μg/kg and the limit of quantification was 0.18 μg/kg. The recoveries were 79.4%-108.7% at 1.0, 5.0 and 10.0 μg/kg, and relative standard deviations(S_(RSD)) were 1.97%-5.85%. The method was simple, rapid and reliable, and could be used for the determination of chloramphenicol in Xuanwei ham.