RP-HPLC法测定狼毒大戟中4种松香烷岩大戟二萜内酯

Determination of four ent-abietane jolkinolides diterpene lactones from Euphorbia fischeriana Steud. by RP-HPLC

目的 建立同时测定狼毒大戟中4种松香烷岩大戟二萜内酯的方法.方法 采用Agilent ZORBAX SB C18色谱柱（4.6mm×250mm,5μm）,以水（A）-乙腈（B）为流动相梯度洗脱[10％～60％B（0～30 min）,60％～85％B（30～50min）,85％ ～100％B（50～55 min）,100％B（55 ～70 min）],体积流量1.0 mL/min；检测波长240 nm,柱温30℃.结果 17-acetoxyjolkinolide A、17-hydroxyjolkinolide B、jolkinolide B和jolkinolide A线性范围分别为0.034 2 ～0.308 2 μg（r=0.999 9）、0.040 8～0.367 0 μg（r=0.999 9）、0.049 9 ～0.448 9 μg（r=0.999 9）和0.022 8 ～0.205 4μg（r=1.000）,平均回收率分别为97.0％ （RSD为0.95％,n=6）、97.0％ （RSD为1.54％,n=6）、96.8％ （RSD为1.50％,n=6）和97.2％ （RSD为1.32％,n=6）.结论 该方法同时测定4种有效成分,结果稳定,重复性好.

AIM To develop an HPLC method for detemining four ent-abietane jolkinolides diterpene lactones from Euphorbiafischeriana Steud. METHODS The column was an Agilent ZORBAX SB-C18s column （4. 6 mm × 250 mm, 5 μm）. The mobile phase consisted of water （A）. and acetonitrile （B）. The HPLC elution condition was optimized as follows： 10% -60% B （0-30 min）, 60% -85% B （30-50 rain）, 85% -100% B （50-55 min）, 100% B （55-75 min）. The flow rate was at 1.0 mL/min. The detection wavelength was set at 240 nm with the column temperature of 30 %. RESULTS The linear range was 0. 034 2-0. 308 2 μg （ r = 0. 999 9） for 17-acetoxyjolkino- lide A with the mean recovery of 97.0% （RSD of 0.95% , n =6）. The linear range was 0. 040 8-0. 367 0 μg （r = 0. 999 9） for 17-hydroxyjolkinolide B with the mean recovery of 97.0% （RSD of 1.54% , n =6）. The linear range was 0. 049 9-0. 448 9 μg （ r = 0. 999 9） for jolkinolide B with the mean recovery of 96. 8% （ RSD of 1.50% , n = 6）. The linear range was 0. 022 8-0. 205 4 p.g （r = 1. 000） for jolkinolide A with the mean recovery of 97.2% （ RSD of 1.32% , n = 6）. CONCLUSION The method is accurate, reproducible, and suitable for the determi- nation of 4 ent-abietane jolkinolide diterpene lactones from Euphorbia fischeriana Steud.