摘要
该试验旨在建立高效液相色谱-串联质谱法快速测定猪肉中硝基咪唑类药物残留。样品用乙腈(含0.2%甲酸)提取,然后经过净化处理,目标物在液相系统进行洗脱分离,并使用质谱电喷雾电离源正扫描模式进行检测。优化了色谱流动相条件以及样品提取液的净化处理方式,在优化条件下,4种硝基咪唑类药物在1.0~25 ng/m L浓度范围内表现出较好的线性关系,相关系数≥0.991;在3个水平(0.25,0.5和2.5μg/kg)的加标试验中,回收率范围和相应的标准偏差(n=6)分别为:76.7%~105.6%,RSD≤13.9%;84.0%~107.1%,RSD≤4.2%;87.8%~102.0%,RSD≤2.5%。该方法具有良好的准确度和精密度,且检出限较低(0.25μg/kg),能够满足日常快速检验的需求。
It was to establish a method for quick determination of nitroimidazoles by high performance liquid chromatographytandem mass spectrometry.The sample was extracted with 0.2%formic acid-acetonitrile solution and purified.The targets were eluted and separated by the chromatographic column,and the electrospray ionization source was used with the positive ion switching mode to detect them.The conditions of chromatographic mobile phase and the purification treatment of sample extraction were optimized.Under the optimal conditions,four kinds of nitroimidazoles had good linear relationships in the range of 1.0-25 ng/m L,and the correlation coefficients were more than 0.991.The recoveries at 3 spiked levels(0.25,0.5 and 2.5μg/kg)were 76.7%-105.6%,84.0%-107.1%and 87.8%-102.0%,respectively;The relative standard deviations(n=6)were RSD≤13.9%,RSD≤4.2%and RSD≤2.5%,respectively.The method,featured by good accuracy,precision and low detection limit(0.25μg/kg),could meet the requirements for rapid detection.
作者
王斌
牛记者
董丹丹
郭柏坤
王莲芳
上官苗苗
WANG Bin;NIU Jizhe;DONG Dandan;GUO Baikun;WANG Lianfang;SHANGGUAN Miaomiao(Hangzhou Yuhang Food and Drug Monitoring&Testing Center,Hangzhou 311199)
出处
《食品工业》
CAS
北大核心
2020年第9期321-325,共5页
The Food Industry
基金
浙江省食品药品监管系统科技计划项目(2019004)“畜禽肉类多药物残留快速筛查技术的研究和应用”。
关键词
硝基咪唑类药物
快速测定
高效液相色谱-串联质谱法
nitroimidazoles
rapid determination
high performance liquid chromatography-tandem mass spectrometry method
