HPLC法测定黄芩素静脉注射亚微乳剂的含量___

目的：建立黄芩素静脉注射亚微乳剂中黄芩素含量测定的高效液相色谱法。方法：采用化学破乳法，以无水乙醇为破乳剂破坏乳剂界面性质，制备供试品溶液；以kromasil C18(5 μm，4.6 mm × 250 mm)为色谱柱，甲醇-0.05%磷酸（65∶35）为流动相，流速1.0 mL·min-1，检测波长275 nm，外标法测定。结果：乳剂中加入50倍无水乙醇可获得澄清透明的供试品溶液；在1.2~48.0 μg·mL-1浓度范围内，峰面积与黄芩素浓度的线性方程为A=56.23C-2.703，r=0.9999；低、中、高浓度连续进样的RSD分别为1.1%，0.23%，0.10%；8 h内样品溶液稳定，样品重复测定的RSD为1.2%；平均回收率为100.7%（n=9）。结论：无水乙醇具有良好的破乳效果，空白乳剂对测定无干扰，方法简便、准确，能够满足黄芩素亚微乳剂中黄芩素含量测定的要求。

Objective：To establish an RP-HPLC method for the determination of baicalein in its submicron for injection.Methods：The analysis was carried on a kromasil C18(5 μm，4.6 mm × 250 mm) column，using methanol-0.05%phosphoric acid（65∶35）as the mobile phase.The detection wavelength was set at 275nm and flow rate was 1.0 mL·min-1.Results：The assay displayed good linearity over the range of 1.2-48 μg·mL-1 and the regression equation obtained was A=56.233C-2.703（r=0.9999）.The precisions（RSD）of the three concentrations（high，medium and low）of baicalein standard solutions were 1.11%,0.23%,0.10%，respectively.Baicalein was stable in the prepared samples after placing in the auto-sampler for 8h at ambient temperature.The repetition RSD of baicalein was 1.2%.The average recovery was 100.7%（n=9）.Conclusion：The method is simple，accurate and suitable for the content determination of baicalein in its submicron emulsion for injection.

1ZHANG Xi-ping（张喜平）,LI Zong-fang（李宗芳）,LIU Xiao-Gong（刘效恭）.Review in pharmacological study of baicalein（黄芩素药理学研究概况）.Chin Pharmacol Bull（中国药理学通报）,2001,17(6):117

2Shinichi Ikemoto，Kazunobu Sugimura，Naomasa Yoshida，et al.Antitumor effects of scutellariae radix and its components baicalein，and wogonin on bladder cell lines.Urol,2000,55(6):951

3YAO Ya-hong(姚亚红)，ZHANG Li-wei（张立伟）.Studies on preparation technique and in vitro release of baicalein liposomes（黄芩素脂质体的制备及体外释放的研究）.Acta Chin Med Pharmacol（中医药学报），2006，34（3）：31

4FU Hong（符洪），XIAO Xin-yue（肖新月），ZHANG Nan-ping（张南平），et al.Determination and chromatogram recognition of main chemical constituents in Radix Scutellariae of different resource（药用黄芩中主要化学成分分析）.Chin J Pharm Anal（药物分析杂志），2003，23（1）：33

5REN Hai-yong（任海勇），ZHANG Zuo-ping（张作平），YI Ying-ping（衣银萍），et al.Determination of baicalein and wogonin in ertong qianlie soft capsule by HPLC(HPLC法测定二酮前列软胶囊中黄芩素与汉黄芩素的含量).Trad Chin Drug Res Clin Pharmacol（中药新药与临床药理），2008，19（5）：384

6LIU Bin（刘斌），SHI Ren-bing（石任兵），JIANG Yan-yan（姜艳艳），et al.HPLC determination of the contents of four flavonoids in effective fraction of kushen decoction (HPLC法测定苦参汤有效部位中4种黄酮类成分含量).J Beijing Univ Trad Chin Med（北京中医药大学学报），2005，28（6）：59

7ZHU Wen-bing（祝文兵）.Determination of bacalein in kangbingdu mixture by RP-HPLC（RP-HPLC测定抗病毒合剂中黄芩素的含量）.China Pharm（中国药师），2008，11（1）：111