摘要
豆芽样品采用pH 4.0的乙二胺四乙酸二钠-Mcllvaine缓冲溶液提取,采用MCX固相萃取柱进行在线净化。采用高效液相色谱-串联质谱法测定样品溶液中15种喹诺酮类药物的残留量。以Waters BEH C18色谱柱为固定相,以不同体积比的0.2%(体积分数,下同)甲酸溶液和0.2%甲酸乙腈溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾电离源正离子模式和多反应监测模式。15种喹诺酮类药物的质量浓度均在5~120μg·L^-1内与其对应的峰面积呈线性关系,检出限(3S/N)为2μg·kg^-1,测定下限(10S/N)为6μg·kg^-1。以空白样品为基体进行加标回收试验,所得回收率为62.0%~89.3%,测定值的相对标准偏差(n=6)为2.4%~11%。
The bean sprout sample was extracted with EDTA-mcllvaine buffer solution of pH 4.0.MCX solid phase extraction column was used as on-line purification.HPLC-MS/MS was applied to the determination of residual amounts of 15 quinolones in the sample solution.Waters BEH C18 chromatographic column was used as stationary phase,and the mixture of 0.2%(φ,the same below)formic acid solution and 0.2%formic acid acetonitrile solution mixed in different ratios was used as mobile phase in gradient elution.ESI+and multi-reactions monitor mode were adopted in MS/MS.Linear relationships between values of peak area and mass concentration of 15 quinolones were kept in the same range of 5-120μg·L^-1,with detection limits(3 S/N)of 2μg·kg^-1 and lower limits of determination(10 S/N)of 6μg·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 62.0%-89.3%,with RSDs(n=6)of determined values in the range of 2.4%-11%.
作者
徐潇颖
赵超群
梁晶晶
周霞
刘柱
XU Xiaoying;ZHAO Chaoqun;LIANG Jingjing;ZHOU Xia;LIU Zhu(Zhejiang Institute for Food and Drug Control,Hangzhou 310052,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2020年第5期583-589,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
浙江省食品药品监管系统科技计划项目(SP201701)。
