GC法测定马香苓口服液中百秋李醇含量研究

Determination of Patchouli Alcohol in Maxiangling Oral Liquid by GC

试验旨在建立测定马香苓口服液中百秋李醇含量的研究方法。本研究采用气相色谱法,其色谱条件是使用色谱柱HP-5毛细管柱;柱温采用程序升温(初始温度150℃,保持18 min,以50℃/min速率升至280℃,保持5 min);进样口温度为280℃;载气:高纯氮气;流速1 mL/min;进样量1μL,分流比20∶1;检测器为氢火焰离子化检测器,温度为280℃;氢气流速40 mL/min,空气流速370 mL/min;分别进行系统适用性试验、专属性试验、线性范围考察、检测限和定量限的确定、精密度试验、稳定性试验、重复性试验、加样回收率试验、耐用性试验,并对10批样品进行了含量测定。结果显示,专属性溶液中的溶剂峰、药液的杂质峰与主成分峰能达到有效分离且分离度符合要求(R≥1.5),表明该方法系统适用性良好;阴性对照溶液未检出色谱峰,表明样品中其他成分不干扰测定;百秋李醇定量限和检测限分别为2.842和0.812μg/mL;百秋李醇检测质量浓度在15.86~1015μg/mL范围内与峰面积积分值呈良好的线性关系(y=0.869x-10.45,R^2=0.999,n=7)。精密度试验、稳定性试验(日内和日间精密度)、重复性试验的平均RSD分别为0.90%、1.63%和1.83%、2.90%,其RSD均在可控范围内(RSD≤3%);平均加样回收率为95.36%,RSD=2.82%(n=6),表明所建立的气相色谱法检测百秋李醇的含量回收率良好;进行耐用性试验,最终验证所建立的色谱方法可以稳定检测百秋李醇的含量。经方法学验证,该方法准确稳定,简便可行,能够作为马香苓口服液君药广藿香中百秋李醇的含量控制方法,同时也为该制剂质量控制提供了一种有效的检测方法,暂定本品中广藿香药材按百秋李醇计不少于47.53μg/mL。

The purpose of the experiment was to establish a capillary gas chromatography(GC)method for the content determination of patchouli alcohol in Maxiangling oral liquid.The samples were determined by capillary GC.The chromatographic conditions were as follows:The chromatographic column HP-5 capillary column was used,and the column temperature was controlled by programming(the initial temperature was 150℃,held for 18 min,and then rose at a rate of 50℃/min up to 280℃for 5 min).The injector temperature was 280℃.Carrier gas was high purity nitrogen.The flow rate was 1 mL/min.The injection volume was 1μL,and the split ratio was 20∶1.FID detector was used and the detector temperature was 280℃.Hydrogen flow rate was 40 mL/min and air flow rate was 370 mL/min.The system applicability test,specificity test,linear range test,determination of detection limit and quantitative limit,precision test,stability test,repeatability test,sample recovery test,durability test and content determination of ten batches of samples were conducted.The results showed that the solvent peak,impurity peak and main component peak in the specific solution could be separated effectively and the resolution of the chromatographic method met the requirements(R≥1.5),which showed that the method had good applicability.No outstanding peak was detected in the negative control solution,indicating that other components in the sample did not interfere with the determination.Limit of quantitation(LOQ)and limit of detection(LOD)of patchouli alcohol were 2.842 and 0.812μg/mL.Under the above chromatographic conditions,a good linearity was obtained in the range of 15.86-1015μg/mL(y=0.869x-10.45,R^2=0.999,n=7);RSDs of precision,stability(intra-day precision and daytime precision)and reproducibility tests were 0.90%,1.63%and 1.83%,2.90%,respectively.RSDs were within controllable range(RSD≤3%).The average recovery was 95.36%,with a RSD of 2.82%(n=6).The results showed that the established gas chromatography method had a good recovery rate for the determination of patchouli alcohol.The durability test was carried out to verify that the established chromatographic method could stably determine the content of patchouli alcohol.The methodological verification showed that the GC method was accurate,stable,convenient and feasible,and could be used as a method for the content control of patchouli alcohol in Maxiangling oral liquid.At the same time,it also provided an effective detection method for the quality control of this preparation.It was tentatively determined that the content of patchouli alcohol in this product was not less than 47.53μg/mL.