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目的:用快原子轰击质谱(FAB-MS)建立一种川芎嗪定量分析的新方法。方法:以氘代甲醇为氘代试剂,激光照射0.5h得到的氘代川芎嗪为内标物;内标物与被测样品分子离子峰总离子流作非线性拟合,其初始峰强的比值与样品浓度呈线性,藉此对样品定量分析。质谱条件:快原子轰击源(FAB),仪器分辨率1000,枪压8kV,原子枪气Ar,底物为甘油。结果:氘代试剂用氘代甲醇,激光照射0.5h下,氘代率为2.43%;以其作内标物,得到川芎嗪定量分析的工作曲线,线性方程为Y=6.75+2.24X(r=0.9908),精密度RSD=2.9%。用此方法对磷酸川芎嗪片剂进行分析,给出了2种不同前处理方法的分析结果43.0mg.片-1和45.0mg·片-1。结论:快原子轰击质谱的非线性拟合法,是一种川芎嗪定量分析的新方法,该方法只需微克级样品,且干扰少,精度高。
Objective: To establish a new method for quantitative analysis of Tetramethylpyrazine with Fast Atom Bombardment Mass Spectrometry (FAB-MS). METHODS: The deuterated methanol was used as the deuterated reagent, and the deuterated Ligustrazine was used as the internal standard after laser irradiation for 0.5 h. The internal standard was nonlinearly fitted with the total ion current of the ionized peak of the sample. The initial peak intensity was strong. The ratio is linear with the sample concentration, whereby the sample is quantitatively analyzed. Mass spectrometry conditions: fast atom bombardment source (FAB), instrument resolution 1000, gun pressure 8 kV, atom gun gas Ar, substrate glycerol. RESULTS: When the deuterated reagent was deuterated in methanol for 0.5 h under laser irradiation, the deuteration ratio was 2.43%. Using it as an internal standard, the working curve of the quantitative analysis of tetramethylpyrazine was obtained. The linear equation was Y=6.75+2.24X(r). = 0.9908), precision RSD = 2.9%. In this method, the tetramethylpyrazine phosphate tablets were analyzed and the analysis results of 2 different pretreatment methods were given: 43.0 mg. tablet-1 and 45.0 mg tablet-1. Conclusion: The non-linear fitting method of fast atom bombardment mass spectrometry is a new method for the quantitative analysis of tetramethylpyrazine. This method requires only microgram samples with less interference and high precision.