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目的建立测定腺梗豨莶中ent-16β,17,18-三羟基贝壳杉烷-19-羧酸、奇壬醇、ent-17,18-二羟基贝壳杉烷-19-羧酸、豨莶苷、ent-16β,17-二羟基贝壳杉烷-19-羧酸含量的高效液相色谱示差折光检测方法(HPLC-RID)。方法以十八烷基硅烷键合相为固定相,流动相为体积分数0.5%甲酸溶液-乙腈(体积比72∶28),示差检测器光学元件温度为40℃,流速为1.0 mL·min-1。结果 5种化合物线性关系良好(r>0.999),ent-16β,17,18-三羟基贝壳杉烷-19-羧酸和ent-17,18-二羟基贝壳杉烷-19-羧酸的线性范围为0.10~0.50 g·L-1,奇壬醇的线性范围为0.50~2.5 g·L-1,豨莶苷的线性范围为0.20~1.0 g·L-1,ent-16β,17-二羟基贝壳杉烷-19-羧酸的线性范围为0.42~2.1 g·L-1;平均加样回收率在98.3%~101.1%内,RSD小于3.5%。结论该方法简便、准确、重复性良好,适用于腺梗豨莶中5种成分的同时测定。
Objective To establish a method for determination of ent-16β, 17,18-trihydroxychuane-19-carboxylic acid, nonyl alcohol, ent-17,18-dihydroxychuvane-19-carboxylic acid, Glycosides, ent-16β, 17-dihydroxychuane-19-carboxylic acid content by high performance liquid chromatography refractive index detection method (HPLC-RID). Methods The octadecylsilane-bonded phase was used as the stationary phase. The mobile phase consisted of 0.5% formic acid and acetonitrile (volume ratio 72:28), the temperature of the differential detector optical element was 40 ℃ and the flow rate was 1.0 mL · min- 1. Results The five compounds showed good linearity (r> 0.999). The linearity of ent-16β, 17,18-trihydroxychuane-19-carboxylic acid and ent-17,18-dihydroxychuvane-19-carboxylic acid The linear range of the behenyl alcohol ranged from 0.10 to 0.50 g · L-1. The linear range of the behenyl alcohol ranged from 0.50 to 2.5 g · L-1. The linear range of the berizine ranged from 0.20 to 1.0 g · L-1. The linear range of hydroxy-kaurene-19-carboxylic acid was 0.42-2.1 g · L-1, and the average recovery was 98.3% -101.1% with a RSD less than 3.5%. Conclusion The method is simple, accurate and reproducible. It is suitable for the simultaneous determination of five components in the glandular stem.