双泵双柱UP-LC/MSMS法对烟熏肉制品中氯霉素、氟苯尼考和甲砜霉素的稳定性分析

Stability analysis of chloramphenicol,florfenicol and thiamphenicol in smoked meat products by double-pump double-column UP-LC/MSMS

建立了双泵双柱高效液相色谱/质谱法对烟熏肉制品中氯霉素、氟苯尼考和甲砜霉的快速分析方法。试样经氨化乙酸乙酯提取,浓缩后用(1+9)乙腈+水定容,正己烷去脂,得到样品待测液。试验结果:氯霉素类在0.5~10.0 ng/mL浓度范围内具有良好线性关系,相关系数均大于0.995;不同浓度加标回收率均在80.2%~109.2%之间,相对偏差小于14.6%:方法检出限为氯霉素0.1μg/kg,甲砜霉素和氟苯尼考0.5μg/kg。在30天周期性质稳定。此方法重现性好,灵敏度高,分析高效、快捷,能满足批量样品快速分析。

The rapid determination method for the stability of chloramphenicol,florfenicol and thiamphenicol in smoked meat products by dual-pump dual-column UP-LC/MSMS was established.The sample was extracted by ammoniated ethyl acetate,concentrated,volume-stabilized by(1+9)acetonitrile and purified water,and degreased by n-hexane before testing.The results showed that the compounds had good linear relationship in the concentration range of 0.5 ng/mL to 10.0 ng/mL,the correlation coefficients were all greater than 0.995,the recoveries of different concentrations were between 80.2%and 109.2%,the relative standard deviations were less than 14.6%.The limit of detection was 0.1μg/kg for chloramphenicol,and 0.5μg/kg for thiamphenicol and florfenicol.In the 30-day cycle,the compounds were stable.The method has the advantages of good reproducibility,high sensitivity,and high efficiency,and can be used for the rapid analysis of large quantities of samples.