HPLC-ELSD法测定麻花秦艽中4种脂溶性成分的含量___

目的: 建立测定麻花秦艽中齐墩果酸、胡萝卜苷、栎瘿酸及β-谷甾醇的蒸发光散射检测-高效液相色谱法。 方法: 采用Kromasil C₁₈(150 mm×4.6 mm,5 μm)色谱柱;流动相:A为乙腈-冰醋酸(99.94∶ 0.06),B为甲醇-冰醋酸(99.94∶ 0.06),梯度洗脱 0);33~60 min,A-B(100∶ 0)→A-B(50∶ 50)];流速为1.0 mL·min^-1;柱温25 ℃;漂移管温度为70 ℃;载气流速为1.7 L·min^-1。 结果: 齐墩果酸、胡萝卜苷、栎瘿酸及β-谷甾醇分离良好,进样量分别在0.31~3.1 μg(r=0.9997)、0.615~6.15 μg(r=0.9998)、0.77~7.7 μg(r=0.9997)、0.66~6.6 μg(r=0.9999)范围内线性关系良好。平均回收率(n=3)分别为99.9%,100.1%,99.8%,100.1%;RSD分别为0.73%,0.41%,0.21%,0.56%。 结论: 本法准确,专属性强,重现性好,可作为麻花秦艽中4种主要脂溶性成分齐墩果酸、胡萝卜苷、栎瘿酸及β-谷甾醇的测定方法。4种脂溶性成分中,含量最高的为栎瘿酸,最高者可达4.71 mg·g^-1,其余成分均约为0.78 mg·g^-1。

Objective: To develop an HPLC-ELSD method for simultaneous determination of four liposoluble components(oleanolic acid,daucosterol,roburic acid,β-sitosterol)in Gentiana straminea Maxim.. Methods: The chromatographic separation was achieved on a Kromasil C₁₈(150 mm×4.6 mm,5 μm)column with mobile phase A 0.06)] and mobile phase B 0.06)] by gradient elution 0);33-60 min,A-B(100∶ 0)→A-B(50∶ 50)].The flow rate was 1.0 mL·min^-1 with column temperature at 25 ℃.The drift-tube temperature of ELSD was 70 ℃,and the flow rate of air was 1.7 L·min^-1. Results: The calibration curves of oleanolic acid,daucosterol,roburic acid,and β-sitosterol were in good linearity over the ranges of 0.31-3.1 μg(r=0.9997),0.615-6.15 μg(r=0.9998),0.77-7.7 μg(r=0.9997),0.66-6.6 μg(r=0.9999),respectively.The recoveries(n=3)of oleanolic acid,daucosterol,roburic acid,β-sitosterol were 99.9%(RSD=0.73%),100.1%(RSD=0.41%),99.8%(RSD=0.21%),100.1%(RSD=0.56%),respectively. Conclusion: The determination results of 8 batch samples showed that the method is easy,accurate and can be used in the determination of four liposoluble components in Gentiana straminea Maxim..Roburic acid has the highest contents in the four liposoluble components,4.71 mg·g^-1,approximately;others are all 0.78 mg·g^-1,approximately.

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