摘要
建立了一种用于化妆品中氯霉素快速检测的实时直接分析-高分辨质谱法。样品以乙醇为提取溶剂超声、振荡萃取,纯水稀释1倍后,采用12 Dip-it Samplers模式进样,在负离子模式下,以全扫描-平行反应监测(Full MS-PRM)模式进行直接定量分析。离子化温度为500℃,进样速度为0.3 mm/s。结果表明,氯霉素在0~100 mg/L范围内具有良好的线性关系,相关系数(r)为0.998 4,方法定量下限(LOQ)为3.0 mg/kg。在3.0、6.0、30 mg/kg 3个加标水平下的回收率为70.2%~119%,相对标准偏差(RSD)为8.4%~17%。该方法具有样品前处理简单、分析速度快、基质干扰小等优点,适用于化妆品中氯霉素的快速检测。
A method for the determination of chloramphenicol in cosmetics was developed using direct real-time analysis-high resolution mass spectrometry.The sample was ultrasonically extracted with ethanol,then diluted 1 ∶1 by volume with water,and finally injected with a 12 Dip-it Samplers.The instrument parameter were optimized to obtain the sensitive and accurate determination for chloramphenicol.At a sample introduction rate of 0.3 mm/s,high intensity of [M-H]^-ions for chloramphenicol were observed in the negative ion and Full MS-PRM mode by utilization of high purity helium gas at 500 ℃.The calibration curve for chloramphenicol was linear in the range of 0-100 mg/L with a correlation coefficient of 0.998 4.The limit of quantitation(LOQ) of the method was 3.0 mg/kg.Recoveries for chloramphenicol at three spiked levels of 3.0,6.0,30 mg/kg were in the range of 70.2%-119%,with relative standard deviations(RSD) of 8.4%-17%.With its rapid analysis,simple pretreatment steps and low matrix interference,the method was suitable for the rapid determination of chloramphenicol in cosmetics.
作者
蓝草
邵琳智
陈思敏
LAN Cao;SHAO Lin-zhi;CHEN Simin(Guangzhou Customs TecUnology Center,Guangzhou 510428,China;Key Laboratory of Animais of Plants and Food Import and Export of Technical Measures in Guangdong Province,Guangzhou 510428,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2019年第12期1503-1506,共4页
Journal of Instrumental Analysis
基金
原广东出入境检验检疫局科技计划项目(2018GDK14).
关键词
实时直接分析
高分辨质谱
化妆品
氯霉素
快速检测
direct analysis in real time
high resolution mass spectrometry
cosmetics
chloramphenicol
rapid determination
