Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n. 15782, Santiago de Compostela, Spain.
J Chromatogr A. 2010 Oct 8;1217(41):6342-9. doi: 10.1016/j.chroma.2010.08.034. Epub 2010 Aug 19.
A simple and fast sample pre-treatment method based on matrix solid-phase dispersion (MSPD) for isolating cocaine, benzoylecgonine (BZE), codeine, morphine and 6-monoacethylmorphine (6-MAM) from human hair has been developed. The MSPD approach consisted of using alumina (1.80 g) as a dispersing agent and 0.6M hydrochloric acid (4 mL) as an extracting solvent. For a fixed hair sample mass of 0.050 g, the alumina mass to sample mass ratio obtained was 36. A previously conditioned Oasis HLB cartridge (2 mL methanol, plus 2 mL ultrapure water, plus 1 mL of 0.2M/0.2M sodium hydroxide/boric acid buffer solution at pH 9.2) was attached to the end of the MSPD syringe for on column clean-up of the hydrochloric acid extract and for transferring the target compounds to a suitable solvent for gas chromatography (GC) analysis. Therefore, the adsorbed analytes were directly eluted from the Oasis HLB cartridges with 2 mL of 2% acetic acid in methanol before concentration by N(2) stream evaporation and dry extract derivatization with N-methyl-tert-butylsilyltrifluoroacetamide (BSTFA) and chlorotrimethylsilane (TMCS). The optimization/evaluation of all the factors affecting the MSPD and on column clean-up procedures has led to a fast sample treatment, and analytes extraction and pre-concentration can be finished in approximately 30 min. The developed method has been applied to eight hair samples from poli-drug abusers and measured analyte concentrations have been found to be statistically similar (95% confidence interval) to those obtained after a conventional enzymatic hydrolysis method (Pronase E).
已开发出一种基于基质固相分散（MSPD）的简单快速的样品预处理方法，用于从人发中分离可卡因、苯甲酰古柯碱（BZE）、可待因、吗啡和 6-单乙酰吗啡（6-MAM）。MSPD 方法包括使用氧化铝（1.80 g）作为分散剂和 0.6M 盐酸（4 mL）作为提取溶剂。对于固定的头发样品质量为 0.050 g，氧化铝与样品的质量比为 36。将先前经过条件处理的 Oasis HLB 柱（2 mL 甲醇，加 2 mL 超纯水，再加 1 mL 0.2M/0.2M 氢氧化钠/硼酸缓冲溶液，pH 值为 9.2）连接到 MSPD 注射器的末端，用于盐酸提取物的柱上净化以及将目标化合物转移到适合气相色谱（GC）分析的溶剂中。因此，吸附的分析物直接从 Oasis HLB 柱上用 2 mL 甲醇中的 2%乙酸洗脱，然后通过 N(2)流蒸发浓缩并通过 N-甲基叔丁基硅基三氟乙酰胺（BSTFA）和三甲基氯硅烷（TMCS）进行干提取物衍生化。对影响 MSPD 和柱上净化程序的所有因素进行了优化/评估，从而实现了快速的样品处理，并且可以在大约 30 分钟内完成分析物的提取和预浓缩。该方法已应用于 8 个来自多药滥用者的头发样本，并发现测量的分析物浓度与使用常规酶解方法（Pronase E）获得的浓度具有统计学上的相似性（95%置信区间）。
