摘要
目的:建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定牛奶样品中6种兽药残留(硝碘酚腈、碘醚柳胺、氯氰碘柳胺、托曲珠利、三氯苯达唑、水杨酸钠)的检测方法。方法:样品经过乙腈溶液提取,以MAX固相萃取柱净化,采用Waters X Bridge BEH C_(18)色谱柱分离,流动相以乙腈和0.1%甲酸水溶液梯度洗脱,并使用电喷雾离子源,正负离子切换扫描模式进行检测,外标法定量。结果:6种兽药在0~10 ng/mL范围内呈现良好的线性关系,决定系数(R2)均大于0.995。6种兽药方法的检出限为0.06~0.18μg/kg,方法的定量限为0.5~2.0μg/kg。在添加量为0.5~8.0μg/kg的加标回收实验下,6种兽药加标回收率为67.1%~105.5%,相对标准偏差均小于10%。结论:该方法前处理操作简便,分析速度快,灵敏度高,可用于牛奶样品中的兽药残留测定。
Objective:To establish a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for the determination of six veterinary drug residues in milk samples.Methods:The sample was extracted with acetonitrile solution,purified with MAX solid phase extraction column,and separated by Waters X Bridge BEH-C_(18)chromatographic column.The mobile phase was eluted with a gradient of acetonitrile and 0.1% formic acid aqueous solution,and electrospray ion source was used,positive and negative ion switching scanning mode for detection,external standard method for quantification.Results:The 6 veterinary drugs showed a good linear relationship in the range of 0~10 ng/mL,and the coefficient of determination(R^(2)) was greater than 0.995.The detection limit of the 6 veterinary drugs was 0.06~0.18 μg/kg.The limit of quantification of the method was 0.5~2.0 μg/kg.With the addition of 0.5~8.0 μg/kg in the standard recovery experiment,the recovery rates of the 6 veterinary drugs were 67.1%~105.5%,and the relative standard deviations were all less than 10%.Conclusion:This method is easy to operate,fast in analysis,and high in sensitivity.It can be used for the determination of veterinary drug residues in milk samples.
作者
张敏
王鸽
马晓冲
张耀广
柴艳兵
李兴佳
李飞
ZHANG Min;WANG Ge;MA Xiaochong;ZHANG Yaoguang;CHAI Yanbing;LI Xingjia;LI Fei(Key Laboratory of Dairy Quality and Safety Control,Ministry of Agriculture and Rural Affairs,Shijiazhuang Junlebao Dairy Co.,Ltd.,Shijiazhuang 050021,China)
出处
《食品工业科技》
CAS
北大核心
2022年第5期255-261,共7页
Science and Technology of Food Industry
基金
国家重点研发计划(2018YFC1604304)
河北省重点研发计划(20327117D)。
关键词
高效液相色谱-串联质谱法
兽药残留
固相萃取
牛乳
high performance liquid chromatography-tandem mass spectrometry
veterinary drug residue
solid phase extraction technology
milk