气相色谱内标法测定松节中α-蒎烯的含量
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摘要
目的:采用气相色谱法对不同来源的松节药材中α-蒎烯含量进行检测,为松节药材的质量控制提供依据。方法:使用ZB-5毛细管柱(30 m×0.25 mm×0.25μm),程序升温,初始温度60℃,保持2 min,以20℃/min速率升温至160℃,再以120℃/min速率升温至260℃,保持2 min。进样口温度200℃,氢焰离子化检测器(FID)温度300℃,进样量1μL,分流比10∶1。用环己酮为内标物,按内标法以峰面积计算含量。结果:α-蒎烯在0.125~4 mg/m L浓度范围内线性关系良好(r=0.9996,n=6),平均加样回收率为103.8%(RSD=0.7%,n=9)。结论:该方法具有灵敏、简便、准确的特点,可对松节药材进行有效的质量控制。
Objective To determine α-pinene content of Chinese pine from different places by gas chromatography,and to provide the basis for the quality control of Chinese pine. Methods The analytical condition was based on ZB-5 capillary column( 30 m ×0. 25 mm × 0. 25 μm) with programmed temperature steps. Temperature programming started at 60℃,holding for 2 min,then increased to 160 ℃ at a rate of 20 ℃/min and increased to 260 ℃ at a rate of 120 ℃/min,holding for 2 min. The temperatures of the inlet and FID detector were 200℃ and 300℃,respectively. The injection volume was 1 μL with the split ratio 10∶ 1. Cyclohexanone was used as the internal standard and the content of α-pinene was calculated by peak area according to internal standard method. Results The linear relationship of α-pinene was excellent over the range of 0. 125 ~ 4 mg/m L( r = 0. 9996,n = 6),and the mean recovery was 103. 8% with RSD of 0. 7%( n = 9). Conclusion The quantitative determination method was sensitive,simpleand reliably and was suitable for the quality control of Chinese pineand its preparations.
Objective To determine α-pinene content of Chinese pine from different places by gas chromatography,and to provide the basis for the quality control of Chinese pine. Methods The analytical condition was based on ZB-5 capillary column( 30 m ×0. 25 mm × 0. 25 μm) with programmed temperature steps. Temperature programming started at 60℃,holding for 2 min,then increased to 160 ℃ at a rate of 20 ℃/min and increased to 260 ℃ at a rate of 120 ℃/min,holding for 2 min. The temperatures of the inlet and FID detector were 200℃ and 300℃,respectively. The injection volume was 1 μL with the split ratio 10∶ 1. Cyclohexanone was used as the internal standard and the content of α-pinene was calculated by peak area according to internal standard method. Results The linear relationship of α-pinene was excellent over the range of 0. 125 ~ 4 mg/m L( r = 0. 9996,n = 6),and the mean recovery was 103. 8% with RSD of 0. 7%( n = 9). Conclusion The quantitative determination method was sensitive,simpleand reliably and was suitable for the quality control of Chinese pineand its preparations.
引文
[1]贵州省药品监督管理局.贵州省中药材、民族药材质量标准[M].贵州:贵州科技出版社,2003:247.
[2]陈曦.HPLC测定松节、松针和松香中银松素和甲基醚的含量[J].天津药学,2014,26(5):21-23.
[3]张林林,薛健,刘东静,等.油松节药材中α-蒎烯的测定方法研究[J].中草药,2009,11:1817-1818.
[4]朱沛韶,陈浩桉,吴翔.松节油中α-蒎烯的测定[J].中药材,1999,22(7):362-363.
[5]国家药典委员会.中华人民共和国药典(一部)[M].北京:中国医药科技出版社,2015:227.
[2]陈曦.HPLC测定松节、松针和松香中银松素和甲基醚的含量[J].天津药学,2014,26(5):21-23.
[3]张林林,薛健,刘东静,等.油松节药材中α-蒎烯的测定方法研究[J].中草药,2009,11:1817-1818.
[4]朱沛韶,陈浩桉,吴翔.松节油中α-蒎烯的测定[J].中药材,1999,22(7):362-363.
[5]国家药典委员会.中华人民共和国药典(一部)[M].北京:中国医药科技出版社,2015:227.