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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。
Objective To establish a method for simultaneous determination of chloramphenicol and thiamphenicol in milk by high performance liquid chromatography-mass spectrometry. Methods The samples were filtered by acetonitrile liquid-liquid extraction and polyethersulfone needle filter, and then separated by gradient elution on a ZORBAX Eclipse Plus C18 column. The single quadrupole mass spectrometer was used for the quantitative analysis by standard curve method. Results The linear regression equations of chloramphenicol and thiamphenicol were y = 82.276x + 141.31 and y = 299.92x + 267.31, respectively. The linear correlation coefficients were all greater than 0.999 in the range of 0.1ng / ml to 100ng / ml. The limits of recovery were 0.25μg / kg and 0.27μg / kg, respectively. The recoveries were 91.3% -97.3% and 89.0% -98.2%, respectively. The relative standard deviations (RSDs) were <5.6%. Conclusion The method is rapid, simple, accurate, sensitive and suitable for the determination of chloramphenicol and thiamphenicol in milk.