高效液相色谱质谱联用法同时测定牛奶中氯霉素、甲砜霉素残留量

目的 建立高效液相色谱-质谱联用同时测定牛奶中氯霉素、甲砜霉素方法。方法 样品经乙腈液-液萃取、聚醚砜针式过滤头过滤后,再经ZORBAX Eclipse Plus C18色谱柱梯度洗脱分离,单四级杆质谱仪检测,标准曲线法定量。结果 氯霉素和甲砜霉素线性回归方程分别为y=82.276x+141.31和y=299.92x+267.31;在0.1ng/ml~100ng/ml范围内,线性相关系数均大于0.999;方法检出限分别为0.25μg/kg和0.27μg/kg;加标回收率分别为91.3%~97.3%和89.0%~98.2%。相对标准偏差(RSD)均＜5.6%。结论 本方法快速、简便、准确、灵敏,适合于牛奶中氯霉素和甲砜霉素的测定。

Determination of Chloramphenicol and Thiamphenicol residue in milk by high-performance liquid chromatography-mass spectrometry

Objective To establish a method of high-performance liquid chromatography-mass spectrometry for the determination of chloramphenicol and thiamphenicol residues in milk.Methods Chloramphenicol and thiamphenicol in milk were extracted with acetonitrile and then filtrated through 0.45μm syringe of polyether sulphone filter.ZORBAX Eclipse Plus C18 column was used for separation,and single quadrupole mass spectrometer was used for qualitative analysis,with standard curves for quantitative analysis.Results In the range from 0.1ng/ml to 100ng/ml,linear regression equations were y=82.276x+141.31 and y=299.2x+267.31 for chloramphenicol and thiamphenicol,respectively.The correlation coefficients were both greater than 0.999.The detection limits were 0.25μg/kg and 0.27μg/kg for chloramphenicol and thiamphenicol,with the recovery rates 91.3%-97.3% and 89.0%-98.2%,respectively.The relative standard deviations (RSDs) were both less than 5.6%.Conclusion The method is fast,convenient,accurate and sensitive and it can be applied for the determination of chloramphenicol and thiamphenicol in milk.