UPLC-UV-MS法应用于胃肠安丸中11个活性成分的定性与定量分析

目的: 建立超高效液相色谱-紫外-串联质谱法应用于胃肠安丸中11个活性成分(川芎嗪、阿魏酸、柚皮苷、橙皮苷、芦荟大黄素、大黄酸、大黄素、和厚朴酚、厚朴酚、大黄酚、大黄素甲醚)的定性、定量分析方法。 方法: 采用ACQUITY UPLC BEH C₁₈(2.1 mm×50 mm, 1.7 μm)色谱柱,以0.1%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱(0~7.5 min,90%A→25%A),流速0.3 mL·min^-1,DAD波长切换检测模式,柱温40℃,进样量2 μL;Waters Quattro Premier XE质谱仪,正/负离子检测模式。 结果: 各成分在7.5 min内分离良好,通过与对照品的保留时间(t_R)和质谱信息的对比,确定了胃肠安丸中的11个活性成分;它们在相应的浓度范围内与峰面积呈良好的线性关系,相关系数均>0.9977;加样回收率(n=5)为96.6%~107.2%,RSD均小于3.0%。批内精密度RSD均小于1.0%,批间精密度RSD均小于3.5%。 结论: 本方法简便、快速、准确,精密度高,重复性好,适用于胃肠安丸中多种活性成分的快速定性、定量分析。

Objective: To develop a simple, efficient and reliable method for simultaneous quantitation and qualitation of eleven compounds(ligustrazine, ferulic acid, naringin, hesperidin, aloe-emodin, rhein, emodin, honokiol, magnolol, chrysophanol, physcion) in Weichangan pills by UPLC-UV-MS. Methods: The chromatographic separation was performed on a Waters ACQUITY UPLC system using an ACQUITY UPLC BEH C₁₈(2.1 mm × 50 mm, 1.7 μm) column. The analysis was accomplished in 7.5 min with a gradient elution of water containing 0.1% formic acid (A) and acetonitrile (B) at flow rate of 0.3 mL·min^-1. The switched wavelength of DAD was employed: 0-1.92 min: 320 nm(ligustrazine, ferulic acid), 1.93-3.00 min: 283 nm(naringin, hesperidin), 3.01-5.50 min: 254 nm(aloe-emodin, rhein), 5.51-6.26 min: 294 nm(emodin, honokiol), 6.27-7.50 min: 254 nm(magnolol, chrysophanol, physcion). The column temperature was set at 40℃. The injection volume was 2 μL. The mass spectra were obtained by Waters Quattro Premier XE mass spectrometer. The positive and negative ion modes were converted to detect the eleven compounds. Results: By comparing with the retention time(t_R) and mass spectrometry fragments data of reference substances, eleven compounds in Weichangan pill were identified. All calibration curves were linear(r>0.9977) over the tested ranges. The average recoveries ranged from 96.6% to 107.2% with RSD value below 3.0%. The RSDs of within-run and between-run precision were below 1.0% and 3.5%, respectively. Conclusions: The method is simple and fast with high precision, sensitivity and repeatability, which can be used for qualitative and quantitative analysis of multi-components in Weichangan pills.