目的 建立高效液相结合一测多评（HPLC-QAMS）法同时测定金果含片中哈巴苷、哈巴俄苷、柚皮芸香苷、橙皮苷、川陈皮素、橘红素、麦冬甲基黄烷酮A和甲基麦冬二氢高异黄酮B的方法。方法 采用Agilent HC C18色谱柱（250 mm×4.6 mm，5 μm），流动相为乙腈-0.05%磷酸溶液，梯度洗脱；检测波长为210 nm（哈巴苷和哈巴俄苷）和296 nm（柚皮芸香苷、橙皮苷、川陈皮素、橘红素、麦冬甲基黄烷酮A和甲基麦冬二氢高异黄酮B）；体积流量1.0 mL/min；进样量10 μL；柱温30℃。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。以橙皮苷为内参物，建立该成分与哈巴苷、哈巴俄苷、柚皮芸香苷、川陈皮素、橘红素、麦冬甲基黄烷酮A和甲基麦冬二氢高异黄酮B的相对校正因子（RCF），并计算金果含片中8种成分的含量，同时与外标法的测定结果进行比较，验证该方法的可行性。结果 哈巴苷、哈巴俄苷、柚皮芸香苷、橙皮苷、川陈皮素、橘红素、麦冬甲基黄烷酮A和甲基麦冬二氢高异黄酮B检测质量浓度的线性范围分别为6.54～163.50、2.27～56.75、8.16～204.00、17.95～448.75、1.88～47.00、0.54～13.50、1.48～37.00和0.76～19.00 μg/mL（r值范围0.999 1～0.999 8）；平均加样回收率及RSD值分别为99.85%（0.76%）、97.62%（1.07%）、100.09%（0.64%）、99.80%（0.71%）、97.48%（1.44%）、98.25%（1.60%）、96.90%（1.03%）、96.87%（1.31%），方法学验证结果均符合要求。HPLC-QAMS法计算值与外标法实测值无显著性差异。结论 所建立的HPLC-QAMS法简便、有效、准确，可用于金果含片中多指标成分含量的同时测定，为提升金果含片的质量控制方法提供参考依据。

Objective To develop an HPLC-QAMS method for simultaneous determination of harpagide, harpagoside, narirutin, hesperidin, nobiletin, tangeretin, methylophiopogonanone A and methylophiopogonanone B in Jinguo Hanpian. Methods The determination was performed on an Agilent HC C18 column(250 mm×4.6 mm, 5 μm) with gradient elution, and the mobile phase consisted of acetonitrile-0.05% phosphoric acid at the flow rate of 1.0 mL/min. The detection wavelengths were set at 210 nm for harpagide and harpagoside, 296 nm for narirutin, hesperidin, nobiletin, tangeretin, methylophiopogonanone A and methylophiopogonanone B. The column temperature was set at 30℃, and the injection volume was 10 μL.Using hesperidin as an internal standard, the relative correction factor (RCF) of harpagide, harpagoside, narirutin, nobiletin, tangeretin, methylophiopogonanone A and methylophiopogonanone B were calculated. The RCFs value were used to calculate the contents of eight components in Jinguo Hanpian, and compared with the results of the external standard method (ESM) to verify the feasibility of the method. Results The linear range was 6.54-163.50 μg/mL for harpagide, 2.27-56.75 μg/mL for harpagoside, 8.16-204.00 μg/mL for narirutin, 17.95-448.75 μg/mL for hesperidin, 1.88-47.00 μg/mLfor nobiletin, 0.54-13.50 μg/mL for tangeretin, 1.48-37.00 μg/mL for methylophiopogonanone A, 0.76-19.00 μg/mL for methylophiopogonanone B (r=0.999 1-0.999 8). The average recovery and RSD were 99.85% (0.76%), 97.62% (1.07%), 100.09% (0.64%), 99.80% (0.71%), 97.48% (1.44%), 98.25% (1.60%), 96.90% (1.03%) and 96.87% (1.31%). Significant difference weren't found between the calculated value of HPLC-QAMS method and the measured value of external standard method. Conclusion The HPLC-QAMS is simple, effective and accurate, which can be used for simultaneous determination of multi-index component in Jinguo Hanpian, and it can provide reference for the increase of quality control method of Jinguo Hanpian.

R927.2

山东省中医药科技发展计划项目（2019-0449）