GC校正因子在黄樟醚、甲基丁香酚定量分析中的应用

Application of GC Calibration Factors in Quantitative Analysis of Safrole and Methyl Eugenol

目的:将GC校正因子应用于细辛中黄樟醚、甲基丁香酚定量分析。方法:首先采用Agilent 6890N气相色谱仪,FID检测器,DB-WAX毛细管柱(250μm×30 m,0.25μm),检测器温度250℃,进样口温度230℃,载气氮气,恒压模式,进样量1μL,流速1.0 m L·min^(-1),氢气流速45 m L·min^(-1),空气流速450 m L·min^(-1),尾吹氮气流速35 m L·min^(-1),温度条件(起始温度135℃保持2 min,以5℃·min^(-1)升至160℃保持7 min,再以20℃·min^(-1)升至220℃保持3 min);再通过不同测定及计算方法得多个GC校正因子值;最后经稳定性、重复性、加样回收率试验验证可行性,筛选校正因子值应用于黄樟醚、甲基丁香酚的定量分析。结果:各校正因子值计算稳定性、重复性试验结果 RSD均<3%;黄樟醚平均加样回收率范围为92.96%~121.35%,RSD 3.4%~4.8%,甲基丁香酚为88.80%~112.54%,RSD 2.0%~3.4%;最终获得应用于10批细辛中黄樟醚、甲基丁香酚定量分析。结论:2个GC校正因子值定量分析10批细辛中黄樟醚、甲基丁香酚结果相差不大,多个GC校正因子值的筛选应用有利于提高实验检测结果的准确性。

Objective： To apply GC calibration factors in quantitative analysis of safrole and methyl eugenol in Asarum. Method： First, Agilent 6890N GC, detector FID, column DB-WAX （250 μm × 30 m, 0.25 μm） were used with detector temperature of 250 ℃ , inlet temperature of 230 ℃ , gas of N2 under constant pressure mode. The flow rate was 1.0 mL · min-1, injection volume of 1 μL, hydrogen flow of 45 mL · min-1 , air flow of 450 mL · min-1, and tail blown nitrogen of 35 mL· min-1 The initial temperature was 135 ℃ for 2 min; rose to 160 ℃ at 5 ℃ · min-1and maintained for 7 min; then rose to 220℃ at 20 ℃ · min-1 and maintained for 3 min. After that, a variety of determination and calculation methods were adopted to obtain a number of GC calibration factor values. Finally, after verification of their feasibility through stability, repeatability and samplerecovery rate tests to screen the calibration factors for quantitative analysis of safrole and methyl eugenol. Result： The values calculated in stability and repeatability tests all had RSDs less than 3% ; the average recoveries were 92.96% -121.35% , with RSDs of 3.4% -4.8% for safrole; and 88.80% -112.54% with RSDs of 2.0% -3.4% for methyl eugenol. Finally, 10 batches of Asarum of safrole and methyl eugenol were determined by two GC calibration factors. Conclusion： Two GC correction factor values did not have many differences for quantitative analysis of safrole and methyl eugenol in Asarum, and the application of various determination and calculation methods of GC calibration factors can improve the accuracy of the test results.