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目的:建立药用辅料间甲酚含量测定的气相色谱分析方法。方法:采用气相色谱法,色谱柱:Agilent DB-225 MS(30m×0.25 mm,0.25μm);升温程序:起始温度为90℃,维持10 min,以每分钟2℃的速率升至120℃,再以每分钟10℃速率升至150℃,维持5 min,进样口温度为200℃,检测器为火焰离子化检测器,温度为250℃。流速为1.8 ml·min-1;分流比为1∶30;载气为氮气。结果:间甲酚在0.6~1.8 mg·ml-1的范围内,其浓度与样品和内标峰面积的比值呈良好线性关系;平均回收率为96.0%,RSD为2.6%(n=9)。三批样品的测量结果分别为99.3%、98.7%和98.4%。结论:所建立的气相色谱法专属性强,准确度高、重复性好,可用于间甲酚的质量控制。
Objective: To establish a gas chromatographic method for the determination of m-cresol in medicinal materials. Methods: Gas chromatography was performed on an Agilent DB-225 MS (30 m × 0.25 mm, 0.25 μm) temperature program. The temperature was raised to 90 ° C for 10 min and the temperature was raised to 120 ° C at a rate of 2 ° C per minute The temperature was raised to 150 ° C at a rate of 10 ° C per minute for 5 minutes. The temperature of the inlet was 200 ° C. The detector was a flame ionization detector at a temperature of 250 ° C. The flow rate was 1.8 ml · min-1; the split ratio was 1:30; the carrier gas was nitrogen. Results: The concentration of m-cresol in the range of 0.6-1.8 mg · ml-1 showed a good linear relationship with the ratio of sample and internal standard peak area. The average recovery was 96.0% and the RSD was 2.6% (n = 9) . Three batches of samples measured results were 99.3%, 98.7% and 98.4%. Conclusion: The established gas chromatography has the advantages of high specificity, high accuracy and good repeatability, and can be used for the quality control of m-cresol.