摘要
目的建立高效液相色谱-串联质谱法(highperformanceliquidchromatography-tandemmass spectrometry,HPLC-MS/MS)测定豆芽中甲硝唑和羟基甲硝唑检测方法。方法样品经乙酸乙酯提取2次,旋转蒸发,混合阳离子交换柱净化,经InfinityLabPoroshell SB-Aq色谱柱分离, HPLC-MS/MS检测,内标法定量分析。结果甲硝唑和羟基甲硝唑在1.0~100.0μg/L范围内线性关系良好,线性相关系数均大于0.998。在1.0、5.0和10.0μg/kg3个添加水平下的平均回收率为83%~105%,相对标准偏差在2.2%~5.5%之间,检出限为0.3μg/kg,定量限为1.0μg/kg。结论该方法灵敏可靠,回收率稳定,适用于豆芽中甲硝唑和羟基甲硝唑的同时测定。
Objective To establish a methodfor the determination of metronidazole andhydroxymetronidazole in bean sproutsbyhigh performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The sample was extracted twice with ethyl acetate,rotary evaporated,purified by a mixed cation exchange column,separated by an InfinityLabPoroshell SB-Aq column,detected by HPLC-MS/MS,and quantitatively analyzed by internal standard method.Results Metronidazole and hydroxymetronidazole had good linear relationships in the range of 1.0-100.0μg/L,and the linear correlation coefficients were both greater than 0.998.The average recoveries at spiked levels of 1.0,5.0 and 10.0μg/kg ranged from 83%-105%,with relative standard deviations(RSD)from 2.2%to 5.5%.The limit of detectionand limit of quantification were 0.3μg/kg and 1.0μg/kg,respectively.Conclusion This method is sensitive and accurate,and has stable recovery rate,which is suitable for simultaneous determination of metronidazole and hydroxymetronidazole in bean sprout.
作者
潘项捷
陆文琪
王璐璐
李云萱
张水锋
PAN Xiang-Jie;LU Wen-Qi;WANG Lu-Lu;LI Yun-Xuan;ZHANG Shui-Feng(Zhejiang Fangyuan Test Group Co.Ltd.,Hangzhou 310018,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2021年第9期3460-3464,共5页
Journal of Food Safety and Quality
基金
国家市场监督管理总局技术保障专项项目(2020YJ014)。
关键词
豆芽
甲硝唑
羟基甲硝唑
高效液相色谱-串联质谱法
bean sprouts
metronidazole
hydroxymetronidazole
high performance liquid chromate graphy-tandem mass spectrometry