摘要
采用超高效液相色谱-串联质谱法测定蜂蜜中甲硝唑的含量。蜂蜜样品经磷酸氢二钾溶液溶解,乙酸乙酯提取,用MCS固相萃取柱净化。以Hypersil Gold-C_(18)色谱柱为分离柱,以不同体积比的0.1%(体积分数)甲酸溶液和乙腈混合液为流动相进行梯度洗脱,采用电喷雾正离子源多反应监测模式检测。以D4-甲硝唑为内标物。甲硝唑的线性范围为0.5~64.0μg·L^(-1),方法的测定下限(10S/N)为0.15μg·kg^(-1)。以空白样品为基体进行加标回收试验,所得回收率在95.6%~98.8%之间,测定值的相对标准偏差(n=6)在4.2%~8.3%之间。
UHPLC-MS/MS was applied to the determination of metronidazole in honey.The sample of honey was dissolved with di-potassium hydrogen phosphate solution,and then extracted with ethyl acetate.The extract was purified with MCS solid phase extraction column.Hypersil Gold-C_（18） chromatographic column was used as stationary phase,and the mixture of 0.1%（φ）formic acid solution and acetonitrile mixed in different ratio was used as mobile phase in gradient elution.ESI^＋ and multi-reactions monitor were adopted in MS/MS.D4-metronidazole was used as internal standard.Linearity range of metronidazole was found between 0.5μg·L^（-1） and 64.0μg·L^（-1）with lower limit of determination（10S/N）of 0.15μg·kg^（-1）.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 95.6%-98.8%,with RSD′s（n=6）in the range of 4.2%-8.3%.
出处
《理化检验（化学分册）》
CSCD
北大核心
2017年第8期946-949,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
