气相色谱内标法测定松节中α-蒎烯的含量

Gas Chromatography Determination of α-Pinene Contentin Chinese Pine by Internal Standard Method

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 in- creased 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. Resuits 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.