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气相色谱内标法测定松节中α—蒎烯的含量

2018-09-18周孟廖祥明王珊杨雄李勇军巩仔鹏张荣红

中国民族民间医药·下半月 2018年3期

周孟 廖祥明 王珊 杨雄 李勇军 巩仔鹏 张荣红

【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 × 0.25 μm),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1 μL,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/mL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。

【关键词】 松节;α-蒎烯;气相色谱法;含量测定

【中图分类号】R284.1 【文献标志码】 A【文章编号】1007-8517(2018)06-0010-05

Abstract:Objective To determine α-pinene content ofChinese 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/mL (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.

Keywords:Chinese pine; α-Pinene; Gas Chromatographic; Content Determination

松节为松科植物云南松(Pinus yunnanensis Franch.)、马尾松(Pinus massoniana Lamb.)的干燥瘤状节,具有祛风燥湿,舒筋活络,活血止痛之功效,可用于关节疼痛,筋骨挛急,脚痹痿软,跌扑瘀诸病[1]。松节入药始载于《名医别录》[2],广泛分布于四川、云南、贵州和广西等地。收载于《贵州省中药、民族药材质量标准》(2003版),但该标准未明确规定其质量控制方法,对不同来源的松节药材中α-蒎烯含量进行含量测定,为松节药材的质量标准提升提供依据,有一定理论意义和实际应用价值。目前对于松树药用价值的研究,主要是针对松花粉、松針、松香和松节油,而对松节的研究较少[3]。α-蒎烯为松节中重要的组成成分之一,也是松节油中主要成分,可用于肌肉痛及关节痛,许多进口药用油均以α-蒎烯含量作为质量指标[4]。中药材一般成分复杂,质量难以把控,然而单一成分含量标准具有较好的可控性和易操作性,为现在最常用的方法之一。……

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