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血浆和尿液中左旋2-羟基-N-环丙基甲基吗啡喃的葡萄糖醛酸苷测定

GLC determination of l-2-hydroxy-N-cyclopropylmethylmorphinan in plasma and urine.

作者信息

Weinfeld R E, Holazo A, Kaplan S A

出版信息

J Pharm Sci. 1976 Dec;65(12):1827-31. doi: 10.1002/jps.2600651232.

Abstract

A specific method was developed for the determination of l-2-hydroxy-N-cyclopropylmethylmorphinan in plasma and urine by GLC, using flame-ionization detection. The method involves the extraction of the compound into ether from plasma or urine at pH 7.4, followed by back-extraction into 1 N HCl. The acid phase is ether washed and made alkaline, and the compound is reextracted into ether. The ether is evaporated to dryness, the residue is dissolved in methanol, and an aliquot is analyzed by GLC. The same method is applicalble to plasma and urine samples following deconjugation of the compound with glucuronidase-sulfatase. The overall recovery is 93.1 +/- 9.4% SD) in the concentration range of 0.020-2.0 microgram/ml. The method was successfully applied to plasma and urine specimens obtained after administering single 25-mg oral doses to humans.

摘要

已开发出一种通过气相色谱法(GLC)并使用火焰离子化检测来测定血浆和尿液中l - 2 - 羟基 - N - 环丙基甲基吗啡喃的特定方法。该方法包括在pH 7.4条件下将化合物从血浆或尿液中萃取到乙醚中,随后反萃取到1N盐酸中。酸相用乙醚洗涤并碱化,然后将化合物重新萃取到乙醚中。将乙醚蒸发至干,残渣溶于甲醇,取一份溶液进行气相色谱分析。在用葡萄糖醛酸酶 - 硫酸酯酶使化合物解共轭后,相同方法适用于血浆和尿液样本。在0.020 - 2.0微克/毫升的浓度范围内,总回收率为93.1±9.4%(标准差)。该方法已成功应用于给人类单次口服25毫克剂量后获得的血浆和尿液样本。

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