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气相色谱/电子轰击电离质谱法测定人血浆中的丙卡特罗

Determination of procaterol in human plasma by gas chromatography/electron impact ionization mass spectrometry.

作者信息

Huang S L, Wang W, Ou-Yang D S, Zhou H H

机构信息

Pharmacogenetics Research Institute, Basic & Clinical Pharmacology Institute, Hu-nan Medical University, Changsha 410078, China.

出版信息

Acta Pharmacol Sin. 2000 Jun;21(6):564-6.

Abstract

AIM

To improve a gas chromatography/electron impact ionization mass spectrometry (GC/MS) method for determining the concentration of procaterol in human plasma.

METHODS

GC/MS was developed with capillary column. Samples were extracted by liquid phase before derivated. Imipramine was used as an internal standard. The injector and GC/MS interface temperatures were set at 280 degrees C and 250 degrees C, respectively. The carrier gas (helium) was 0.8 mL.min-1, and injections were made in the pulse-splitless mode. The MS source and MS Quad temperature were 230 degrees C and 150 degrees C, respectively.

RESULTS

The detection limit of plasma procaterol was 5 ng.L-1. The assay was linear over the range of 10-10,000 ng.L-1 with correlation coefficient of 0.9987. The coefficients of variation were less than 10% for procaterol detection at high, medium and low concentration levels (n = 5). The average recovery of the assay was 99.1% +/- 1.3%.

CONCLUSION

This assay was sensitive, precise, and accurate for evaluating the clinical pharmacokinetics of procaterol.

摘要

目的

改进气相色谱/电子轰击电离质谱法(GC/MS)以测定人血浆中丙卡特罗的浓度。

方法

采用毛细管柱建立GC/MS方法。样品在衍生前通过液相萃取。以丙咪嗪作为内标。进样口和GC/MS接口温度分别设定为280℃和250℃。载气(氦气)流速为0.8 mL·min⁻¹,进样采用脉冲不分流模式。质谱源温度和质谱四极杆温度分别为230℃和150℃。

结果

血浆中丙卡特罗的检测限为5 ng·L⁻¹。该测定法在10 - 10,000 ng·L⁻¹范围内呈线性,相关系数为0.9987。高、中、低浓度水平(n = 5)下丙卡特罗检测的变异系数均小于10%。该测定法的平均回收率为99.1%±1.3%。

结论

该测定法对于评估丙卡特罗的临床药代动力学具有灵敏性、精密度和准确性。

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