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目的:建立5-单硝酸异山梨酯(5-ISMN)血药浓度测定的气相色谱方法。方法:血样在pH7.8的碱性条件下用二氯甲烷一次提取,然后用HP6890型气相色谱仪进行测定,内标为对硝基苯乙腈。柱温150℃,检测器温度250℃,载气流速48.8ml/min,分流比50∶1。结果:线性方程为:y=0.0138+0.0013576C(r=0.9997,n=7)。线性范围:20～2000ng/ml。血浆中最低检测浓度为5ng/ml。方法回收率高、中、低浓度分别为102.64％±2.88％、96.47％±2.15％和102.12％±2.08％。结论:本文建立的气相色谱-电子捕获检测法(GC-ECD),准确度、灵敏度均高,精密度好,可用于5-ISMN的血药浓度测定。
Objective: To establish a gas chromatographic method for the determination of isosorbide 5-mononitrate (5-ISMN) in plasma. Methods: The blood samples were extracted once with dichloromethane at pH7.8 and then determined by gas chromatograph HP6890 with p-nitrophenyl acetonitrile as the internal standard. The column temperature was 150 ℃, the detector temperature was 250 ℃, the carrier gas flow rate was 48.8ml / min and the split ratio was 50:1. Results: The linear equation was: y = 0.0138 + 0.0013576C (r = 0.9997, n = 7). Linear range: 20 ~ 2000ng / ml. The lowest plasma concentration of 5ng / ml. The recovery rate of the method was 102.64% ± 2.88%, 96.47% ± 2.15% and 102.12% ± 2.08%, respectively. Conclusion: The gas chromatography-electron capture detection (GC-ECD) established in this paper has the advantages of high accuracy and high sensitivity, and good precision. It can be used for the determination of 5-ISMN in plasma.