目的 建立高效液相一測多評(píng)（HPLC-QAMS）法測定鼻炎片中羧基蒼術(shù)苷、蒼術(shù)苷、連翹酯苷B、連翹酯苷A、連翹苷、升麻素苷、升麻素、5-O-甲基維斯阿米醇苷和亥茅酚苷。方法 以乙腈-0.2%磷酸為流動(dòng)相，梯度洗脫，體積流量1.0 mL/min；Agilent HC-C₁₈（250 mm×4.6 mm，5 μm）色譜柱，柱溫30℃；檢測波長203 nm（測定羧基蒼術(shù)苷和蒼術(shù)苷）、275 nm（測定連翹酯苷B、連翹酯苷A和連翹苷）和254 nm（測定升麻素苷、升麻素、5-O-甲基維斯阿米醇苷、亥茅酚苷）。進(jìn)行專屬性試驗(yàn)、線性關(guān)系考察、精密度試驗(yàn)、穩(wěn)定性試驗(yàn)、重復(fù)性試驗(yàn)、加樣回收率試驗(yàn)；以連翹苷為內(nèi)參物，建立該成分與羧基蒼術(shù)苷、蒼術(shù)苷、連翹酯苷B、連翹酯苷A、升麻素苷、升麻素、5-O-甲基維斯阿米醇苷、亥茅酚苷間的相對(duì)校正因子，并計(jì)算鼻炎片中9種成分的含量，同時(shí)與外標(biāo)法（ESM）的測定結(jié)果進(jìn)行比較，驗(yàn)證該方法的可行性。結(jié)果 建立了鼻炎片中9種成分的定量控制方法，方法學(xué)驗(yàn)證結(jié)果符合要求。鼻炎片中各成分的計(jì)算值與實(shí)測值無顯著性差異。結(jié)論 HPLC-QAMS法適用于鼻炎片的多指標(biāo)成分質(zhì)量評(píng)價(jià)模式，可以為鼻炎片質(zhì)量控制方法的建立提供參考。

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

山東省中醫(yī)藥科技發(fā)展計(jì)劃項(xiàng)目（2019-0938）