健步消肿止痛油成分分析与评价

Component Analysis and Evaluation of Jianbu Xiaozhong Zhitong Oil

目的建立分析健步消肿止痛油成分的气相色谱-质谱联用(GC-MS)法,评价其主要成分的稳定性。方法色谱柱为DB-1ms石英毛细管柱(30 m×0.25 mm,0.25μm),进样口温度为250℃,接口温度为260℃,载气为氦气,流速为1.0 mL/min,柱压为80 kPa,分流比为20∶1,进样量为1.0μL,程序升温;采用电子轰击离子源,电离电压为1.2 kV,扫描范围40~400 aum(间歇0.5 s)。采用峰面积归一化法计算各成分的相对百分含量。考察室温敞口放置(48 h)、加热破坏(60℃、2 h)、光照破坏(分别在254 nm和366 nm紫外光灯下各照射2 h)及室温放置(36个月)条件下样品中主要成分的含量,分析其变化规律。结果精密度、稳定性和重复性试验结果的RSD均小于3.0%。共鉴定21个成分,总相对百分含量>98%。α-蒎烯、β-蒎烯、α-松油烯、伞花烃、β-水芹烯、1,8-桉叶素、异龙脑、龙脑、薄荷醇、丁香酚、石竹烯为主要成分,其总相对百分含量>95%。室温敞口放置、加热破坏、光照破坏条件下11个主要成分含量均无明显变化;室温放置36个月,11个主要成分中9个无明显变化,α-松油烯和伞花烃互相消长,但总相对百分含量无明显变化。结论所建立的方法操作简便,结果稳定可靠,可为健步消肿止痛油的质量评价提供参考;健步消肿止痛油的主要成分在室温放置(短期、长期)、加热、光照条件下基本稳定。

Objective To establish a gas chromatography-mass spectrometry(GC-MS)method for analyzing the components of Jianbu Xiaozhong Zhitong Oil,and to evaluate the stability of its main components.Methods The chromatographic column was the DB-1ms quartz capillary column(30 m×0.25 mm,0.25µm),the inlet temperature was 250℃,the interface temperature was 260℃,the carrier gas was helium,the flow rate was 1.0 mL/min,the column pressure was 80 kPa,the split ratio was 20∶1,the injection volume was 1.0µL,and the temperature was programmed.The electron impact ion source was adopted,the ionization voltage was 1.2 kV,the scanning range was 40-400 aum(interval of 0.5 s).The peak area normalization method was used to calculate the relative percentage content of each component.The content of the main components in the samples under conditions of exposure at room temperature(48 h),heating damage(60℃for 2 h),lighting damage(at wavelengths of 254 nm and 366 nm under ultraviolet lamp,each wavelength for 2 h)and storage at room temperature(36 months)was determined to analyze the changes of content.Results The RSDs of the precision,stability and repeatability tests were all lower than 3.0%.A total of 21 components were identified,and their total relative percentage content was higher than 98%.There were 11 main components,includingα-pinene,β-pinene,α-terpinene,cymene,β-phellandrene,1,8-cineole,isoborneol,borneol,menthol,eugenol,caryophyllene,and their total relative percentage content was higher than 95%.There was no significant change in the content of the 11 main components under conditions of exposure at room temperature,heating and lighting damage.After storage at room temperature for 36 months,there was no significant change in the content of nine of the 11 main components,and the relative percentage content ofα-terpinene and cymene showed mutual increase and decrease,while there was no significant change in their total relative percentage content.Conclusion The established method is easy,stable and reliable,which can provide a reference for the quality evaluation of Jianbu Xiaozhong Zhitong Oil.The contents of main components of Jianbu Xiaozhong Zhitong Oil are basically stable under conditions of short-term and long-term storage at room temperature,heating and lighting damage.