SPE-HPLC测定风湿骨痛片中6种生物碱类物质的含量

Content Determination of Six Alkaloids in Fengshigutong Tablet by SPE-HPLC

关键词:  风湿骨痛片  生物碱  固相萃取  高效液相色谱法

Key words:  Fengshigutong tablet  alkaloids  SPE  HPLC

摘要:

目的 建立SPE-HPLC同时检测风湿骨痛片中6种生物碱类物质含量的方法。方法 采用Welch XB-C₁₈（4.6 mm×250 mm，5 μm）色谱柱，以含乙腈-四氢呋喃（25：15）溶液为流动相A，以0.05%醋酸铵溶液为流动相B进行梯度洗脱，流速为1.0 mL·min^-1，检测波长为235 nm，柱温为30℃，进样量为10 μL。结果 6种生物碱在优化条件下均可有效分离，苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、次乌头碱和乌头碱分别在162.4~8 121 ng（r=1.000 0）、24.96~1 248 ng（r=1.000 0）、58.03~2 902 ng（r=1.000 0）、17.26~863.0 ng（r=1.000 0）、20.16~1 008 ng（r=1.000 0）和19.90~995.0 ng（r=1.000 0）内有良好的线性关系，平均回收率为88%~98%，RSD为1.8%~2.4%。结论 该方法准确、可靠，适用于风湿骨痛片中生物碱类物质含量的分析。

Abstract:

OBJECTIVE To establish an SPE-HPLC method for the determination of six alkaloids in Fengshigutong tablet. METHODS Welch XB-C₁₈ column(4.6 mm×250 mm, 5 μm) was used, the mobile phase was a mixture of acetonitriletetrahydrofuran (25:15) (A)-0.05%ammonium acetate at a flow rate of 1.0 mL·min^-1 for gradient elution, the column temperature was 30℃ with analysis was monitored at 235 nm, injection volume 10 μL. RESULTS The good linearity with peak areas was achieved in the rang of 162.4-8 121 ng(r=1.000 0), 24.96-1 248 ng(r=1.000 0), 58.03-2 902 ng(r=1.000 0), 17.26-863.0 ng(r=1.000 0), 20.16-1 008 ng(r=1.0000) and 19.90-995.0 ng(r=1.000 0) for benzoyl new aconitine, benzoyl aconitine, benzoyl methacholine, new aconitine, hypaconitine and aconitine, the average recoveries in the range of 88%-98%, RSD was 1.8%-2.4%. CONCLUSION The method is accurate and reliable, and it is suitable for the analysis of alkaloids content in Fengshigutong tablets.