摘要
该文利用液相色谱-串联质谱建立了同时检测虾肉中安眠酮、地西泮、诺氟沙星以及氧氟沙星的分析方法,并且用此分析方法探究这4种兽药的热稳定性。虾肉样品用乙腈和无水硫酸钠提取,经过C18固相萃取柱净化,以Eclipse XDB-C18柱分离,在正离子模式下用多反应监测模式进行数据采集,基质外标法进行定量。此外,在90℃水浴加热条件下,对4种兽药进行热稳定性研究,加热15、30、45、60 min后,以该文建立的分析方法进行检测。4种兽药在0.05~40 ng/mL线性范围内,相关系数R^(2)均大于0.99,检出限为0.01~0.38μg/kg,4种化合物的回收率为78%~119%,相对标准偏差为1.14%~4.76%。该方法灵敏度高、准确性好,适用于虾肉中安眠酮、地西泮、诺氟沙星以及氧氟沙星的同时检测,并且研究表明,这4种兽药具有良好的热稳定性,在水煮加热过程中不会分解或者转化。
An analytical method was established to simultaneously determine methaqualone,diazepam,norfloxacin,and ofloxacin in shrimp by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)and the thermal stability of the four veteri-nary drugs were studied.The samples were extracted with a mixture of anhydrous sodium sulfate and acetonitrile and purified by C18 car-tridge solid-phase extraction(SPE).Eclipse XDB-C18 column(2.1 mm×150 mm,3.5μm)was utilized to separate analytes.All vet-erinary drug detection was performed on multiple reaction monitoring(MRM)mode in the positive ion mode and the matrix external stand-ard method was for quantification.Furthermore,under the condition of 90℃water bath heating,the thermal stability of the four veterina-ry drugs was studied.After heating for 15,30,45,and 60 min,the analytical method established in this research was used for detection.Results demonstrated that all four veterinary drugs had satisfactory linearity in the concentration range of 0.05-40 ng/mL with correlation coefficients greater than 0.99.The limits of detection(LOD)were between 0.01μg/kg and 0.38μg/kg.The average recovery rate was 78%-119%and the relative standard deviation was1.14%-4.76%.This method is sensitive and accurate,which is suitable for the simultaneous detection of methaqualone,diazepam,norfloxacin,and ofloxacin in shrimp.Moreover,the four veterinary drugs have satis-factory thermal stability,and will not decompose or transform during heating.
作者
沈可伊
邹晓霜
王军
SHEN Keyi;ZOU Xiaoshuang;WANG Jun(College of Food Science&Nutritional Engineering,China Agricultural University,Beijing 100083,China)
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2022年第22期263-268,共6页
Food and Fermentation Industries
基金
北京市科技计划项目(Z191100004019019)。
关键词
高效液相色谱-串联质谱
诺氟沙星
氧氟沙星
安眠酮
地西泮
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
norfloxacin
ofloxacin
methaqua-lone
diazepam
