Salem M Y, Ross S A, Murphy T P, ElSohly M A
National Center for the Development of Natural Products, Research Institute of Pharmaceutical Sciences, University of Mississippi, University 38677, USA.
J Anal Toxicol. 2001 Mar;25(2):93-8. doi: 10.1093/jat/25.2.93.
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%.
需要一种用于提取胎粪样本中 heroin 和代谢物以进行气相色谱 - 质谱联用（GC - MS）分析的方法，该方法应能检测到低水平的这些分析物。因此，对固相萃取（SPE）柱在样品制备中的有效性进行了评估。使用了四种不同类型的市售萃取柱。使用这些 SPE 柱从胎粪样本中提取 heroin、6 - 单乙酰吗啡（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，都测定了提取效率、线性范围、检测限（LOD）、定量限（LOQ）、批间精密度和批内精密度。尽管使用这四种不同类型的 SPE 柱都获得了令人满意的结果，但按照此处概述的程序使用 Clean Screen 柱时观察到了最佳的整体性能。可待因的 LOD 低至 20 ng/g，吗啡为 10 ng/g，6 - MAM 为 2.5 ng/g，可待因的 LOQ 低至 20 ng/g，吗啡为 10 ng/g，6 - MAM 为 5 ng/g。在所有情况下，可待因、吗啡和 6 - MAM 在较宽的浓度范围内（分别为 100 - 2000、100 - 2000 和 5 - 100）均观察到线性关系（r => 0.99）。在 50 ng/g 的可待因和吗啡以及 10 ng/g 的 6 - MAM 水平下，使用这些柱进行分析的精密度显示变异系数范围为 4.75%至 15.5%。
