RP-HPLC法测定注射用丹参酮Ⅱ_A磺酸钠含量和有关物质

HPLC determination of content and related substances of sodium tanshinone Ⅱ_A sulfonate for injection

目的:建立丹参酮Ⅱ_A 磺酸钠制剂的高效液相色谱含量测定方法和有关物质检查方法。方法:采用 C_(18)柱(6.0mm×150mm,5μm),流动相 A 相为20mmol·L^(-1)磷酸二氢钾(含0.5%三乙胺,磷酸调节 pH 至4.0)-甲醇(20:80),B 相为20mmol·L^(-1)磷酸二氢钾(含0.5%三乙胺,磷酸调节 pH 至4.0)-甲醇(80:20),梯度洗脱,流速1.0mL·min^(-1),检测波长为271nm。结果:丹参酮Ⅱ_A 磺酸钠与有关物质分离良好,辅料不干扰测定,方法线性范围1.6～39.2μg·mL^(-1)(r=0.9999),最低检测限10ng·mL^(-1),回收率99.1%(n=9),精密度(RSD)为0.44%(n=6)。结论:方法操作简便准确,灵敏度高,适用于丹参酮Ⅱ_A 磺酸钠制剂的含量测定和有关物质检查。

Objective：To establish an HPLC method for the determination of content and related substances of sodium tanshinone Ⅱ A sulfonate for injection. Method：A ClsCOlumn （6.0 mm × 150 mm,5 μm）was used with the gradient elution using 20 mmol · L^- 1 KH2 PO4 （containing 0. 5 % triethyl amine, adjusted to pH 4.0 using H3PO4） - methanol （20： 80） and 20 mmol · L^ - 1 KH2 PO4 （ containing 0. 5 % triethyl amine, adjusted to pH 4. 0 using H3 PO4 ） - methanol（80： 20） as mobile phase at a flow rate of 1.0 mL · min^-1 and the detection wavelength of 271 nm. Results：The sodium tanshinone Ⅱ A sulfonate and related substances could be basehne separated, and excipient didn＇ t disturb the determination. The calibration curve was linear in the range of 1.6 - 39.2 μg · mL^- 1 （ r = 0. 9999）. The detection limit was 10 ng · mL^-1, average recovery was 99. 1% （ n = 9 ）, precision （RSD） was 0. 44% （n = 6）. Conclusion：This method is rapid, accurate sensitive and can be used for determination of the content and related substances of sodium tanshinone Ⅱ A sulfonate preparation.