目的 建立高效液相一测多评（HPLC-QAMS）法测定鼻炎片中羧基苍术苷、苍术苷、连翘酯苷B、连翘酯苷A、连翘苷、升麻素苷、升麻素、5-O-甲基维斯阿米醇苷和亥茅酚苷。方法 以乙腈-0.2%磷酸为流动相，梯度洗脱，体积流量1.0 mL/min；Agilent HC-C₁₈（250 mm×4.6 mm，5 μm）色谱柱，柱温30℃；检测波长203 nm（测定羧基苍术苷和苍术苷）、275 nm（测定连翘酯苷B、连翘酯苷A和连翘苷）和254 nm（测定升麻素苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷）。进行专属性试验、线性关系考察、精密度试验、稳定性试验、重复性试验、加样回收率试验；以连翘苷为内参物，建立该成分与羧基苍术苷、苍术苷、连翘酯苷B、连翘酯苷A、升麻素苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷间的相对校正因子，并计算鼻炎片中9种成分的含量，同时与外标法（ESM）的测定结果进行比较，验证该方法的可行性。结果 建立了鼻炎片中9种成分的定量控制方法，方法学验证结果符合要求。鼻炎片中各成分的计算值与实测值无显著性差异。结论 HPLC-QAMS法适用于鼻炎片的多指标成分质量评价模式，可以为鼻炎片质量控制方法的建立提供参考。

Objective To develop a HPLC-QAMS method for simultaneous determination of carboxyatractyloside, atractyloside, forsythoside B, forsythoside A, forsythin, prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside and sec-Oglucosylhamaudol in Biyan Tablets. Methods The analysis was carried out on an analytical columnAgilent HC-C₁₈ (4.6 mm×250 mm, 5 μm) with gradient elution by acetonitrile and 0.2% phosphoric acid solution, at the detection wavelength of 203, 275 and 254 nm and a flow rate of 1.0 mL/min; the column temperature was 30 ℃. Using forsythin as an internal standard, the RCFs of carboxyatractyloside, atractyloside, forsythoside B, forsythoside A, prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside and sec-O-glucosylhamaudol were calculated. The RCFs value were used to calculate the contents of nine components in Biyan tablets, and compared with the results of the external standard method (ESM) to verify the feasibility of the method. Different chromatographic columns were used to determine the relative retention time,and the feasibility and accuracy of one test and multiple assessment method for the determination of nine components in Biyan tablets were evaluated. Results The method for quantitative control of nine components in Biyan Tablets was established, and the validation results met the requirements. There was no significant difference between the calculated values and the measured values of nine active components in Biyan tablets. Conclusion The HPLC-QAMS is suitable for the multi-index component quality evaluation mode of Biyan tablets, which can provide reference for the establishment of quality control method of Biyan Tablets.

R284.1

山东省中医药科技发展计划项目（2019-0938）