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超高效液相色谱法测定海洛因及堿性杂质用于药物分析。

Determination of heroin and basic impurities for drug profiling by ultra-high-pressure liquid chromatography.

机构信息

U.S. Drug Enforcement Administration, Special Testing and Research Laboratory, 22624 Dulles Summit Court, Dulles, VA 20166, USA.

出版信息

Forensic Sci Int. 2013 Sep 10;231(1-3):300-5. doi: 10.1016/j.forsciint.2013.06.008. Epub 2013 Jul 6.

DOI:10.1016/j.forsciint.2013.06.008
PMID:23890653
Abstract

Rapid, precise, accurate, and reproducible methodology using ultra-high-pressure liquid chromatography (UHPLC) for the analysis of heroin and basic impurities is described. The determination of heroin, morphine, O3-monoacetylmorphine, O6-monoacetylmorphine, codeine, acetylcodeine, noscapine, and papaverine is accomplished using reversed-phase chromatography (RPC), employing a 1.7 μm Acquity UPLC BEH C18 column (2.1 mm × 150 mm) with a phosphate buffer (pH 1.6)-acetonitrile gradient and PDA detection. The target analytes are well resolved from each other and most adulterants in less than 20 min. For the few instances when adulterants interfere with target analytes, a 1.7 μm Acquity CSH Fluoro-Phenyl (2.1 mm × 150 mm) column is utilized with the same gradient conditions. The reported methodology can detect impurities as low as 0.02% relative to heroin, and is well suited for heroin profiling.

摘要

本文描述了一种使用超高效液相色谱(UHPLC)快速、准确、精确且可重现的方法,用于分析海洛因和碱性杂质。采用反相色谱(RPC),使用 1.7μm Acquity UPLC BEH C18 柱(2.1mm×150mm),以磷酸缓冲液(pH 1.6)-乙腈梯度洗脱和 PDA 检测,实现了海洛因、吗啡、O3-单乙酰吗啡、O6-单乙酰吗啡、可待因、乙酰可待因、那可丁和罂粟碱的测定。目标分析物彼此之间以及大多数杂质在不到 20 分钟的时间内得到很好的分离。对于少数杂质干扰目标分析物的情况,采用相同的梯度条件,使用 1.7μm Acquity CSH Fluoro-Phenyl(2.1mm×150mm)柱。所报道的方法可以检测到相对于海洛因低至 0.02%的杂质,非常适合海洛因分析。

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