固相萃取-超高效液相色谱-串联质谱测定凉茶中15种植物源性兴奋剂和外源性药物

发布时间：2018-01-21 06:02

本文关键词： 凉茶兴奋剂药物超高效液相色谱-串联质谱法固相萃取　出处：《分析化学》2016年10期 　论文类型：期刊论文

【摘要】：建立了固相萃取富集净化,超高效液相色谱-串联三重四级杆质谱(UPLC-MS/MS)测定凉茶中5种植物源性兴奋剂和10种外源性消炎镇痛类药物的方法。样品经高速离心后用甲酸调节至p H 4.0,HLB固相萃取柱净化,BEH C18色谱柱分离,乙腈-0.1%甲酸梯度洗脱,串联质谱电喷雾正、负离子扫描,多反应监测(MRM)模式检测,外标法定量。结果表明,15种待测物在1.0~200μg/L范围内线性关系良好;方法检出限(S/N=3)为0.1~2.0μg/L;添加水平为2.0~100μg/L时,平均回收率为76.4%~107%,相对标准偏差(RSD,n=6)为2.8%~9.7%,日间精密度为2.7%~12.0%。本方法前处理过程简单,净化效果好,灵敏度高,适用于凉茶中植物源性兴奋剂和外源性西药的检测。
[Abstract]:Solid phase extraction (SPE) enrichment and purification were established. Ultra High performance liquid Chromatography-tandem Triple Quaternary Mass Spectrometry (UPLC-MS / MS). Five kinds of plant-derived stimulants and 10 kinds of exogenous anti-inflammatory and analgesic drugs in herbal tea were determined. The samples were adjusted to pH 4.0 with formic acid after high speed centrifugation. HLB solid-phase extraction column was used to purify BEH C18 column, acetonitrile-0.1% formic acid gradient elution, tandem mass spectrometry electrospray positive, negative ion scanning and multi-reaction monitoring. The results showed that there was a good linear relationship in the range of 1.0 ~ 200 渭 g 路L ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1). Methods the detection limit S / N ~ (3) was 0.1 渭 g / L; When the addition level was 2.0 ~ 100 渭 g 路L ~ (-1), the average recovery was 76.410 ~ (7) and the relative standard deviation (RSDN ~ (6)) was 2.8% or 9.7%. The precision of this method is 2.70.The method is simple in pretreatment, good in purifying effect and high in sensitivity. It is suitable for the detection of plant-derived stimulants and exogenous western medicines in herbal tea.
【作者单位】：广州质量监督检测研究院国家加工食品质量监督检验中心(广州)广州市食品安全检测技术重点实验室广州市食品安全风险动态监测与预警研究中心;中国广州分析测试中心;
【基金】：广东省质监局科技计划项目(No.2015CZ13) 广州市质监局科技计划项目(No.2015kj01)资助
【分类号】：O657.63;TS275.2
【正文快照】： 1引言凉茶是汉族中草药植物性饮料的通称,具有清热解毒、润燥解暑的功效,深受国内南方家庭的喜爱。国食药监办[2008]85号“含兴奋剂目录所列物质的中药品种名单”中列出了克仑特罗、氢氯噻嗪等7种兴奋剂,其中植物源性兴奋剂包括士的宁、麻黄碱、吗啡、普拉雄酮、可待因5种。凉

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