HPLC-ELSD法测定注射用银杏二萜内酯中银杏内酯A、B、C、K

Determination of ginkgolide A, B, C, and K in Diterpene Lactones from Ginkgo biloba for injection by HPLC-ELSD

目的建立测定注射用银杏二萜内酯中银杏内酯A、B、C、K的HPLC-ELSD法。方法采用HPLC-ELSD法,Phenomenex Luna C18色谱柱（250 mm×4.6 mm,5μm）,流动相为四氢呋喃–甲醇–水,梯度洗脱;体积流量为1.0 mL/min;柱温为30℃;漂移管温度为105℃,氮气体积流量为3.0 L/min。结果注射用银杏二萜内酯中银杏内酯A、B、C、K分别在1.70-8.50μg（r=0.999 7）、2.45-12.5μg（r=0.999 8）、0.30-1.50μg（r=0.999 7）、0.25-1.25μg（r=0.999 7）呈良好的线性关系;平均回收率分别为101.03%、100.86%、100.78%、101.02%,RSD值分别为0.87%、0.29%、1.30%、1.34%。结论该方法简便准确,重复性好,可用于注射用银杏二萜内酯中银杏内酯A、B、C、K的测定。

Objective To establish the method for determination of ginkgolide A, B, C, and K in Diterpene Lactones from Ginkgo biloba for injection by HPLC-ELSD. Methods HPLC-ELSD method was adopted. Phenomenex Luna C18 column（250 mm × 4.6 mm, 5 μm） was adopted with mobile phase consisted of tetrahydrofuran – methanol – water in gradient elution. The flow rate was 1.0 mL/min. The temperature of column and drift tube was set at 30 and 105 ℃, respectively. The flow rate of gas maintained at 3.0 L/min. Results The liner ranges of ginkgolide A, B, C, and K were 1.70 — 8.50 μg/mL（r=0.999 7）, 2.45 — 12.5 μg/mL（r=0.999 8）, 0.30 —1.50 μg/mL（r=0.999 7）, and 0.25 — 1.25 μg/mL（r=0.999 7）; The average recoveries were 101.03%, 100.86%, 100.78%, and 101.02%, with RSD values of 0.87%, 0.29%, 1.30%, and 1.34%（n=6）, respectively. Conclusion The method could be used for the determination of ginkgolide A, B, C, and K in Diterpene Lactones from Ginkgo biloba for injection with a good sensitivity, accuracy, and reproducibility.