[柱切换高效液相色谱法测定尿液中的吗啡和O6-单乙酰吗啡]

[Column-switching high-performance liquid chromatographic method for the determination of morphine and O6-monoacetylmorphine in urine].

作者信息

Zhang Yu-rong, Wang Rong, Zhang Cheng-gong

机构信息

Shanghai Institute of Forensic Science, Shanghai 200083.

出版信息

Fa Yi Xue Za Zhi. 2002 May;18(2):89-91.

PMID:12596597

Abstract

OBJECTIVE

To develop a column-switching high-performance liquid chromatographic method for the determination of morphine and O6-monoacetylmorphine in urine.

METHODS

Urine samples (1.0 ml) were spiked with 1.0 ml borate buffer, after centrifugation, 1.0 ml of supernate were injected directly into an extraction column (YWG C18 33 mm x 5.0 mm, 10 microns). After a washing step with the extraction mobile phase, the retained morphine and O6-monoacetylmorphine were flushed into the analytical column (Lichrospher 100 CN 125 mm x 4.0 mm, 5 microns) with the mobile phase CH3OH-H2O (60:40). The analytical mobile phase is CH3OH-phosphate buffer (pH6.86) (22:78). The UV detector was set at lambda 286 nm.

RESULTS

The method shows excellent linearity from 50 to 1,600 ng/ml for morphine and from 100 to 1,600 ng/ml for O6-monoacetylmorphine. The linear correlation coefficients were > 0.999. The relative standard deviations were < 4%. The limits of detection were 40 ng/ml for both morphine and O6-monoacetylmorphine.

CONCLUSION

The method described is sensitive, rapid, reproducible, and simple.

摘要

目的

建立一种柱切换高效液相色谱法测定尿液中的吗啡和O6 - 单乙酰吗啡。

方法

取1.0 ml尿液样品，加入1.0 ml硼酸盐缓冲液，离心后，取1.0 ml上清液直接注入萃取柱（YWG C18 33 mm×5.0 mm，10微米）。用萃取流动相洗涤后，保留的吗啡和O6 - 单乙酰吗啡用甲醇 - 水（60:40）流动相冲洗至分析柱（Lichrospher 100 CN 125 mm×4.0 mm，5微米）。分析流动相为甲醇 - 磷酸盐缓冲液（pH6.86）（22:78）。紫外检测器设定波长为286 nm。