UPLC法同时测定丹参片中11个水溶性和脂溶性成分的含量

目的：采用UPLC法同时测定丹参片中11个水溶性和脂溶性成分丹参素钠、二氢丹参酮、隐丹参酮、丹参酮、丹参酮Ⅱ_A、熊果酸、原儿茶醛、迷迭香酸、紫草酸、丹酚酸B和丹酚酸A的含量。方法：采用Waters ACQUITY UPLC C₈色谱柱（2.1 mm×100 mm，1.7 μm），以0.1%磷酸水溶液（A）-乙腈（B）为流动相，梯度洗脱（0~13 min，5% B→22% B；13~16 min，22% B→40% B；16~20 min，40% B→53% B；20~39 min，53% B→80% B），流速0.3 mL·min^-1；检测波长280 nm，柱温20℃，样品管理器温度4℃。结果：丹参素钠、二氢丹参酮、隐丹参酮、丹参酮、丹参酮Ⅱ_A、熊果酸、原儿茶醛、迷迭香酸、紫草酸、丹酚酸B和丹酚酸A进样量分别在0.203 1~8.125、0.035 8~1.431、0.063 3~2.531、0.091 8~3.671、0.090 2~3.606、0.096 1~3.844、0.036 0~1.439、0.158 1~6.324、0.103 1~4.125、0.283 1~11.325和0.191 2~7.647 μg的范围内与色谱峰峰面积呈良好线性关系；平均回收率（n=6）分别为99.2%、99.7%、99.8%、98.9%、99.5%、99.4%、99.6%、99.5%、98.7%、99.3%和98.9%，RSD分别为0.49%、0.44%、0.19%、0.61%、0.63%、0.29%、0.79%、0.48%、0.92%、0.40%和0.88%。8个厂家74批丹参片样品中上述11个成分含量范围分别为0.645~7.182、0.079~1.281、0~2.21、0.109~3.37、0.203~3.063、2.033~3.527、0~1.063、1.354~5.677、1.046~3.909、32.759~51.588、0.156~9.472 mg·g^-1。结论：所建立的方法可作为丹参片的质量控制方法。

Objective:To establish an UPLC method for simultaneous determination of 11 water soluble and lipophilic components including danshensu sodium, dihydrotanshinone, cryptotanshinone, tanshinone, tanshinone Ⅱ_A, ursolic acid, protocatechuic aldehyde, rosmarinic acid, lithospermic acid, salvianolic acid B and salvianolic acid A in Danshen tablets. Methods:The sepatation was performed on Waters ACQUITY UPLC C₈ column (2.1 mm×100 mm, 1.7 μm) with the mobile phase consisting of 0.1% phosphoric acid aqueous (A) -acetonitrile (B) by gradient elution (0-13 min, 5%B→22%B;13-16 min, 22%B→40%B;16-20 min, 40%B→53%B;20-39 min, 53%B→80%B) at a flow rate of 0.3 mL·min^-1. The column temperature was 20℃ and the sample manager temperature was 4℃. The detection wavelength was 280 nm. Results:The linear ranges of danshensu sodium, dihydrotanshinone, cryptotanshinone, tanshinone, tanshinone Ⅱ_A, ursolic acid, protocatechuic aldehyde, rosmarinic acid, lithospermic acid, salvianolic acid B and salvianolic acid A were 0.203 1-8.125, 0.035 8-1.431, 0.063 3-2.531, 0.091 8-3.671, 0.090 2-3.606, 0.096 1-3.844, 0.036 0-1.439, 0.158 1-6.324, 0.103 1-4.125, 0.283 1-11.325 and 0.191 2-2.296 μg, respectively. The recoveries (n=6) of the above-mentioned components were 99.2%, 99.7%, 99.8%, 98.9%, 99.5%, 99.4%, 99.6%, 99.5%, 98.7%, 99.3% and 98.9%, respectively, and the relative standard deviations were 0.49%, 0.44%, 0.19%, 0.61%, 0.63%, 0.29%, 0.79%, 0.48%, 0.92%, 0.40% and 0.88%, respectively. The content ranges of above-mentioned component in 74 batches of samples from 8 manufactures were 0.645-7.182, 0.079-1.281, 0-2.21, 0.109-3.37, 0.203-3.063, 2.033-3.527, 0-1.063, 1.354-5.677, 1.046-3.909, 32.759-51.588 and 0.156-9.472 mg·g^-1, respectively. Conclusion:The method can be used for quality control of Danshen tablets.

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