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首页> 外文期刊>Journal of Analytical Toxicology >GC-MS determination of heroin metabolites in meconium: evaluation of four solid-phase extraction cartridges.
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GC-MS determination of heroin metabolites in meconium: evaluation of four solid-phase extraction cartridges.

机译：GC-MS测定胎粪中海洛因代谢物：评估四个固相萃取柱。

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摘要

A procedure for extraction of heroin and metabolites for gas chromatography-mass spectrometry (GC-MS) analysis of meconium specimens that would allow detection of these analytes at low levels was needed. Solid-phase extraction (SPE) cartridges were therefore evaluated for their effectiveness in sample preparation. Four different types of commercially available extraction cartridges were used. Heroin, 6-monoacetylmorphine (6-MAM), morphine, and codeine were extracted from meconium samples using these SPE cartridges and then simultaneously analyzed using GC-MS. In each case, the extraction efficiency, linearity range, limit of detection (LOD), limit of quantitation (LOQ), between-run precision, and within-run precision were determined. Although satisfactory results were obtained with the four different types of SPE cartridges, best overall performance was observed using Clean Screen columns following the procedures outlined here. LODs as low as 20 ng/g for codeine, 10 ng/g for morphine, and 2.5 ng/g for 6-MAM were obtained, and LOQs as low as 20 ng/g for codeine, 10 ng/g for morphine, and 5 ng/g for 6-MAM were obtained. In all cases linearities were observed (r = > 0.99) for codeine, morphine, and 6-MAM over a wide concentration range (100-2000, 100-2000, and 5-100, respectively). At 50 ng/g codeine and morphine and 10 ng/g 6-MAM, the precision of analysis using these cartridges showed coefficients of variation ranging from 4.75% to 15.5%.
机译：需要一种用于海牛粪标本的气相色谱-质谱（GC-MS）分析的海洛因和代谢物的提取方法，该方法可以检测低含量的这些分析物。因此评估了固相萃取（SPE）柱在样品制备中的有效性。使用了四种不同类型的市售提取盒。使用这些SPE小柱从胎粪样品中提取海洛因，6-一乙酰基吗啡（6-MAM），吗啡和可待因，然后使用GC-MS同时进行分析。在每种情况下，都要确定萃取效率，线性范围，检测限（LOD），定量限（LOQ），批间精密度和批内精密度。尽管使用四种不同类型的SPE小柱获得了满意的结果，但按照此处概述的步骤使用Clean Screen色谱柱可观察到最佳的整体性能。 LODs低至可待因20 ng / g，吗啡10 ng / g和6-MAM 2.5 ng / g，可待因的LOQ低至20 ng / g，吗啡10 ng / g和对于6-MAM，获得5 ng / g。在所有情况下，在很宽的浓度范围内（分别为100-2000、100-2000和5-100）观察到可待因，吗啡和6-MAM的线性（r => 0.99）。在50 ng / g可待因和吗啡和10 ng / g 6-MAM时，使用这些色谱柱的分析精度显示变异系数为4.75％至15.5％。

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