Dell D, Wendt G, Bucheli F, Trautmann K H
J Chromatogr. 1985 Nov 8;344:125-36. doi: 10.1016/s0378-4347(00)82013-7.
A sensitive and selective high-performance liquid chromatographic method for the determination of pyrrolidinone (I) in plasma is described. Compound I was extracted from plasma with methylene chloride using kieselguhr as aqueous phase support. The gamma-aminobutyric acid (II) formed after alkaline hydrolysis of I was derivatised with o-phthalaldehyde, chromatographed on a reversed-phase column, and quantified by fluorescence detection. The limit of quantification was 2.5 ng/ml (intra-assay R.S.D. 5%) using a 1-ml plasma sample. The inter-assay precision was 3-14% (R.S.D.) over the concentration range 2000-5 ng/ml, and the recovery from plasma was quantitative (99.3 +/- 2.9%). The accuracy of this method was established from the good agreement between the values obtained after the analysis of plasma samples by both this method and a gas chromatography--mass spectrometry method. The high-performance liquid chromatographic procedure was applied to the determination of (a) endogenous I in human plasma samples and (b) I in plasma following intravenous administration of this substance to a dog. In twelve human subjects, endogenous concentrations of I of 8.3 +/- 2.3 ng/ml (gas chromatography--mass spectrometry method: 6.1 +/- 2.6 ng/ml) were found.
本文描述了一种灵敏且具选择性的高效液相色谱法，用于测定血浆中的吡咯烷酮（I）。化合物I以硅藻土为水相载体，用二氯甲烷从血浆中萃取。I经碱性水解后生成的γ-氨基丁酸（II）用邻苯二甲醛衍生化，在反相柱上进行色谱分离，并用荧光检测法定量。使用1 ml血浆样品时，定量限为2.5 ng/ml（批内相对标准偏差5%）。在2000 - 5 ng/ml的浓度范围内，批间精密度为3 - 14%（相对标准偏差），血浆回收率为定量（99.3±2.9%）。该方法的准确性通过此方法与气相色谱 - 质谱法分析血浆样品后所得值之间的良好一致性得以确立。高效液相色谱法被应用于测定：（a）人血浆样品中的内源性I；（b）给一只狗静脉注射该物质后血浆中的I。在12名人类受试者中，发现内源性I的浓度为8.3±2.3 ng/ml（气相色谱 - 质谱法：6.1±2.6 ng/ml）。
