超声萃取-三氟乙酰胺衍生化气相色谱-质谱法测定血液中阿片类毒品

发布时间：2018-05-30 12:58

本文选题：气相色谱-质谱法 + 超声萃取　；参考：《理化检验(化学分册)》2009年12期

【摘要】：在pH 9的磷酸盐缓冲介质中,人血试样(其中加乙基吗啡为内标)用氯仿、异丙醇及正庚烷(50+17+33)的混合溶剂进行超声萃取10 min,使其中吗啡、6-单乙酰吗啡和可待因进入有机相。离心分离,取上清液常温下吹干。残渣溶于乙酸乙酯中并用MBTFA试剂进行衍生化,取经衍生化的溶液1μL作气相色谱-质谱测定。人体血液中吗啡、6-单乙酰吗啡、可待因的检出限(3S/N)分别为1,2,3μg·L~(-1),标准曲线线性范围均为10～1 000μg·L~(-1)。1 mL血液中添加10,100,1 000 ng 3个浓度药物,平均相对回收率吗啡为82.4%～85.5%,6-单乙酰吗啡为95.7%～99.1%,可待因为97.5%～101.2%。相对标准偏差(RSD,n=5),RSD_(日内)为4.1%～11.2%,RSD_(日间)为4.9%～12.1%。
[Abstract]:In a phosphate buffer medium of pH 9, human blood samples (with ethylmorphine as internal standard) were extracted by ultrasonic extraction with chloroform, isopropanol and n-heptane 50 17 33 for 10 min, in which morphine 6 monoacetylmorphine and codeine entered into the organic phase. Centrifuge separation, take supernatant to blow dry at room temperature. The residue was dissolved in ethyl acetate and derivatized with MBTFA reagent, and 1 渭 L of the derivative solution was determined by gas chromatography-mass spectrometry. The detection limit of morphine 6-monoacetylmorphine and codeine in human blood was 3s / N, respectively. The calibration curve was linear in the range of 101000 渭 g / L ~ (-1) ~ (-1) 渭 g / L ~ (-1). The average relative recovery of morphine was 82.4 渭 g / L ~ (-1) ~ (-1) ng ~ (-1). The average relative recovery of morphine was 82.44 渭 g / L ~ (-1) and that of codeine was 95.7 渭 g / L ~ (99. 1), and that of codeine was 97.5 渭 g / L ~ (-1) 路mL ~ (-1). The average relative recovery of morphine was 82.44 渭 g / L ~ (-1) 渭 g / L ~ (-1) ~ (-1). The relative standard deviation (RSD) is 4.1and 11.2in the day.
【作者单位】：中国人民公安大学刑事科学技术系;康师傅控股有限公司;
【基金】：北京市教育委员会重点实验室建设计划项目资助(JD100410669)
【分类号】：D919.2

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