[关键词]
[摘要]
目的 建立HPLC-ELSD法同时测定10个批次西黄丸中11-羰基-β-乳香酸、11-羰基-β-乙酰乳香酸、α-乳香酸、β-乳香酸、3-乙酰基-α-乳香酸、3-乙酰基-β-乳香酸6种乳香酸类成分的定量方法。方法 采用HPLC-ELSD法,Waters Symmetry C18色谱柱(250 mm×4.6 mm,5 μm),甲醇-0.5%醋酸水溶液为流动相,梯度洗脱,体积流量为0.8 mL/min,柱温为30℃,漂移管温度45℃,载气为高纯N2,载气体积流量为1.5 L/min。结果 11-羰基-β-乳香酸、11-羰基-β-乙酰乳香酸、α-乳香酸、β-乳香酸、3-乙酰基-α-乳香酸、3-乙酰基-β-乳香酸分别在0.10~3.00 μg(r=0.999 5)、1.23~36.9 μg(r=0.999 5)、0.16~4.80 μg(r=0.999 7)、0.25~7.58 μg(r=0.999 7)、0.21~6.18 μg(r=0.999 5)、0.30~9.00 μg(r=0.999 6)线性关系良好;6种成分的平均回收率(RSD)分别为99.6%(3.70%)、99.1%(3.62%)、99.2%(1.66%)、98.2%(1.89%)、99.1%(3.42%)和99.5%(2.32%),10批西黄丸中6种乳香酸的总量分别为35.1 mg/g(2.08%)、127.8 mg/g(2.10%)、31.3 mg/g(1.74%)、56.2 mg/g(1.64%)、56.5 mg/g(1.61%)、87.8 mg/g(1.73%)。结论 本方法简便、准确、分离效果好,为西黄丸的物质基础研究提供依据。
[Key word]
[Abstract]
Objective To establish an HPLC-ELSD method for simultaneous determination of six kinds of boswellic acids including 11-carbonyl-β-boswellic acid, acetyl-11-carbonyl-β-boswellic acid, α-boswellic acid, β-boswellic acid, 3-acetyl-α-boswellic acid, and 3-acetyl-β-boswellic acid in 10 batches of Xihuang Pill (XHP). Methods The separation was achieved on a Waters Symmetry C18 column (250 mm×4.6 mm, 5 μm) with the mobile phase consisting of methanol-0.5% acetic acid to be gradient elution. Flow rate was 0.8 mL/min and column temperature was 30℃. The samples were tested on Evaporative Light-scattering Detector with drift tube temperature of 45℃, carrier gas of purity N2, and carrier gas flow rate of 1.5 L/min. Results 11-Carbonyl-β-boswellic acid, acetyl-11-carbonyl-β-boswellic acid, α-boswellic acid, β-boswellic acid, 3-acetyl-α-boswellic acid, and 3-acetyl-β-boswellic acid had good linearity in the ranges of 0.10-3.00 μg (r=0.999 5), 1.23-36.9 μg (r=0.999 5), 0.16-4.8 μg (r=0.999 7), 0.25-7.5 μg (r=0.999 7), 0.21-6.3 μg (r=0.999 5), and 0.30-9.0 μg (r=0.999 6), respectively. The average recoveries of the six boswellic acids were 99.6% (3.70%), 99.1% (3.62%), 99.2% (1.66%), 98.2% (1.89%), 99.1% (3.42%), and 99.5% (2.32%), respectively. Conclusion This method is simple, reliable, and with good effect for the separation, and can provide the reference for study on XHP material basis.
[中图分类号]
[基金项目]
广东省科技计划项目(2016A020226031);广州市科技计划项目(201607010334);青年英才培育项目(A1-AFD015131Z08)