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目的:建立HPLC替代对照品法同时测量连翘中连翘酯苷A和连翘苷的含量。方法:选取连翘苷作为连翘含量测定对照品连翘酯苷A的替代对照品,在不同条件下测定替代对照品相对对照品的校正因子,利用校正因子和替代对照品连翘苷进行连翘中连翘酯苷A的含量测定。色谱条件:采用Agilent ZORBAX SB-C18(2)(5μm,4.6 mm×250 mm)色谱柱,以乙腈(A)-0.3%的醋酸水溶液(B)为流动相,梯度洗脱[0～5 min,A-B(15∶85)→A-B(17∶83);5～10 min,A-B(17∶83)→A-B(20∶80);10～15 min,A-B(20∶80)→A-B(23∶77);15～20 min,A-B(23∶77)→A-B(25∶75)],流速0.8 mL·min-1,柱温25℃,检测波长230 nm。结果:连翘酯苷A和连翘苷进样浓度分别在0.08～0.62 mg·mL-1(r=0.9995)和0.012～0.08 mg·mL-1(r=0.9995)内与峰面积呈良好的线性关系,测得校正因子f=0.4761,用替代对照测定方法测得回收率(n=6)为99.20%。结论:本法使用替代对照品法测定了连翘中连翘酯苷A的含量,结果证明了替代对照品法用于连翘药材质量控制可行、实用。
Objective: To establish HPLC alternative reference substance method for the simultaneous determination of Forsythiaside A and forsythin in Forsythia. Methods: Forsythin was used as a substitute of Forsythiaside A (Forsythia suspense) in the determination of Forsythia suspense, and the calibration factor of the substitute reference substance was determined under different conditions. The calibration factor was replaced by the forsythin Determination of Forsythiaside A in Curcuma. Chromatographic conditions: a gradient of acetonitrile (A) -0.3% acetic acid in water (B) was used as a mobile phase with an Agilent ZORBAX SB-C18 (2) (5 μm, 4.6 mm × 250 mm) , AB (15:85) → AB (17:83); 5-10 min, AB (17:83) → AB (20:80); 10-15 min, AB The flow rate was 0.8 mL · min-1. The column temperature was 25 ℃ and the detection wavelength was 230 nm. RESULTS: The concentrations of forsythoside A and forsythin in the samples were 0.08-0.62 mg · mL-1 (r = 0.9995) and 0.012-0.08 mg · mL-1 (r = 0.9995) The linear relationship was measured with a correction factor f = 0.4761 and the recovery (n = 6) was 99.20% with the alternative control assay. Conclusion: This method was used to determine the content of forsythiaside A in Forsythia suspensa by using the reference substance method. The results showed that the alternative reference substance method was feasible and practical for the quality control of forsythia.