采用液相色谱-电喷雾电离质谱联用技术测定尿液中的麦角酰二乙胺（LSD）和N-去甲基麦角酰二乙胺（N-demethyl-LSD）

Determination of LSD and N-demethyl-LSD in urine by liquid chromatography coupled to electrospray ionization mass spectrometry.

作者信息

Hoja H, Marquet P, Verneuil B, Lotfi H, Dupuy J L, Lachâtre G

机构信息

Department of Pharmacology and Toxicology, University Hospital, Limoges, France.

出版信息

J Chromatogr B Biomed Sci Appl. 1997 May 9;692(2):329-35. doi: 10.1016/s0378-4347(97)00008-x.

DOI:10.1016/s0378-4347(97)00008-x

PMID:9188821

Abstract

A sensitive and highly specific method for the determination of LSD and N-demethyl-LSD in urine, using combined liquid chromatography and mass spectrometry (LC-MS) with electrospray ionization, has been developed. Extrelut-3 extraction cartridges were used for a basic sample clean-up. Elution was obtained by toluene-diethyl ether (60:40, v/v). A Nucleosil C18 (150 X 1 mm I.D.) reversed-phase column was used for the chromatographic separation, together with a mixture of 2 mM ammonium formate buffer (pH 3) and acetonitrile (70:30, v/v) as mobile phase. Recoveries were 93 and 80%, detection limits 0.025 and 0.035 ng/ml for LSD and N-demethyl-LSD, respectively. Intra-assay precision, studied at four concentrations, was better than 9% at the ng/ml range and better than 14% at 0.10 ng/ml for both compounds. Limits of quantitation were 0.05 and 0.10 ng/ml for LSD and N-demethyl-LSD, respectively. Reproducibility was good and linearity excellent for LSD in the range from 0.05 to 20 ng/ml (r>0.9999, n=7).

摘要

已开发出一种灵敏且高度特异的方法，用于测定尿液中的麦角酸二乙酰胺（LSD）和N-去甲基-LSD，该方法采用液相色谱-质谱联用（LC-MS）并结合电喷雾电离技术。使用Extrelut-3萃取柱对样品进行碱性净化处理。用甲苯-乙醚（60:40，v/v）进行洗脱。采用Nucleosil C18（150×1 mm内径）反相柱进行色谱分离，以2 mM甲酸铵缓冲液（pH 3）和乙腈（70:30，v/v）的混合物作为流动相。LSD和N-去甲基-LSD的回收率分别为93%和80%，检测限分别为0.025和0.035 ng/ml。在四个浓度水平下研究的批内精密度，对于这两种化合物，在ng/ml范围内优于9%，在0.10 ng/ml时优于14%。LSD和N-去甲基-LSD的定量限分别为0.05和0.10 ng/ml。LSD在0.05至20 ng/ml范围内的重现性良好且线性极佳（r>0.9999，n = 7）。