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尿液中苯丙胺的定量分析:固相萃取、聚合物试剂衍生化及反相高效液相色谱法

Quantification of amphetamine in urine: solid-phase extraction, polymeric-reagent derivatization and reversed-phase high-performance liquid chromatography.

作者信息

Fisher D H, Bourque A J

机构信息

Department of Medical Laboratory Science, Northeastern University, Boston, MA 02115.

出版信息

J Chromatogr. 1993 Apr 21;614(1):142-7. doi: 10.1016/0378-4347(93)80233-t.

DOI:10.1016/0378-4347(93)80233-t
PMID:8496274
Abstract

The concentration of amphetamine was determined in urine using solid-phase extraction, polymeric-reagent derivatization, and reversed-phase high-performance liquid chromatography with ultraviolet detection. To remove a majority of acidic and neutral compounds in urine, a solid-phase extraction was first performed on a sample spiked with the internal standard, 1-methyl-3-phenyl-propylamine. Because amphetamine has a relatively low molar absorptivity, the base was derivatized with a polymeric 1-hydroxybenzotriazole reagent containing a 3,5-dinitrobenzoate active ester. The limit of detection is 14 ng/ml, and the limit of quantification is 47 ng/ml. The calibration curve is linear from 0.01 to 4.0 micrograms/ml. The pooled relative standard deviation is +/- 5.5% for eight urine samples measured in duplicate. The average relative error (bias) is +2.2% when compared to gas chromatography-mass spectrometry.

摘要

采用固相萃取、聚合物试剂衍生化以及带有紫外检测的反相高效液相色谱法测定尿液中苯丙胺的浓度。为去除尿液中的大部分酸性和中性化合物,首先对添加了内标1-甲基-3-苯基丙胺的样品进行固相萃取。由于苯丙胺的摩尔吸光率相对较低,用含有3,5-二硝基苯甲酸活性酯的聚合物1-羟基苯并三唑试剂对碱进行衍生化。检测限为14 ng/ml,定量限为47 ng/ml。校准曲线在0.01至4.0微克/毫升范围内呈线性。对八个尿液样品进行双份测定时,合并相对标准偏差为±5.5%。与气相色谱-质谱联用相比,平均相对误差(偏差)为+2.2%。

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