【摘要】 目的建立高效液相色谱-串联质谱（HPLC-MS/MS）同时测定心通口服液（XOL）中阿魏酸、二苯乙烯苷、葛根素、毛蕊异黄酮苷、柚皮苷、原儿茶醛、丹酚酸B、淫羊藿苷、丹参酮Ⅱ_A、辛弗林的方法。方法采用Phenomenex Luna-C₁₈色谱柱（250 mm×4.6 mm,5μm）;乙腈-甲醇-0.02 mol/L乙酸铵溶液为流动相,梯度洗脱,体积流量为0.9 mL/min。质谱条件:ESI源,采用多反应监测模式（MRM）,以定量离子对峰面积进行定量。结果阿魏酸、二苯乙烯苷、葛根素、毛蕊异黄酮苷、柚皮苷、原儿茶醛、丹酚酸B、淫羊藿苷、丹参酮Ⅱ_A、辛弗林10种成分的线性范围分别为15.22¹5 220 ng/mL（r=0.999 3）、19.52¹9 520 ng/mL（r=0.999 4）、25.41²5 410 ng/mL（r=0.999 5）、35.27³5 270 ng/mL（r=0.999 2）、30.28³0 280 ng/mL（r=0.999 4）、50.11⁵0 110 ng/mL（r=0.999 3）、20.33²0 330 ng/mL（r=0.999 2）、25.22²5 220ng/mL（r=0.999 6）、25.36²5 360 ng/mL（r=0.999 3）、30.29³0 290 ng/mL（r=0.999 2）,平均加样回收率分别为98.15%、101.84%、99.86%、101.08%、100.52%、100.67%、100.46%、99.43%、100.81%、98.37%,RSD分别为1.04%、0.98%、0.75%、0.87%、1.31%、1.27%、1.64%、1.48%、0.67%、1.16%。10批样品中10种指标成分质量浓度分别为0.294⁰.319 mg/mL、0.640⁰.665 mg/mL、4.671⁴.699 mg/mL、0.244⁰.264 mg/mL、2.211².231 mg/mL、0.180⁰.201 mg/mL、0.306⁰.324mg/mL、1.540¹.564 mg/mL、0.504⁰.522 mg/mL、0.809⁰.829 mg/mL。结论该法分离度好,高效快速,可用于XOL的质量控制。更多还原

【Abstract】 Objective To establish an HPLC-MS/MS method for the simultaneous determination of ferulic acid, tetrahydroxystilbene glucoside, puerarin, calycosin-7-glucoside, naringin, protocatechuic aldehyde, salvianolic acid B, icariin, tanshinone Ⅱ_A, and synephrine in Xintong Oral Liquid（XOL）. Methods The analysis was performed on Phenomenex Luna-C₁₈ column（250 mm × 4.6 mm, 5 μm） by gradient elution of acetonitrile-mehanol-0.02 mol/L ammonium acetate. The flow rate was 0.9 mL/min. MS conditions: electrospray ionization（ESI） and multiple reaction monitoring（MRM） were adopted, the detected peak areas of ion pairs were used for quantitative determination. Results The linear ranges of ferulic acid, tetrahydroxystilbene glucoside, puerarin, calycosin-7-glucoside, naringin, protocatechuic aldehyde, salvianolic acid B, icariin, tanshinone Ⅱ_A, and synephrine were 15.22—15 220（r = 0.999 3）, 19.52—19 520（r = 0.999 4）, 25.41—25 410（r = 0.999 5）, 35.27—35 270（r = 0.999 2）, 30.28—30 280（r = 0.999 4）, 50.11—50 110（r = 0.999 3）, 20.33—20 330（r =0.999 2）, 25.22—25 220（r = 0.999 6）, 25.36—25 360（r = 0.999 3）, and 30.29—30 290 ng/mL（r = 0.999 2）. The average recoveries（n = 6） were 98.15%（RSD = 1.04%）, 101.84%（RSD = 0.98%）, 99.86%（RSD = 0.75%）, 101.08%（RSD = 0.87%）, 100.52%（RSD =1.31%）, 100.67%（RSD = 1.27%）, 100.46%（RSD =1.64%）, 99.43%（RSD =1.48%）, 100.81%（RSD = 0.67%）, and 98.37%（RSD =1.16%）, respectively. The contents of 10 batches of the 10 active components were 0.294—0.319, 0.640—0.665, 4.671—4.699, 0.244—0.264, 2.211—2.231, 0.180—0.201, 0.306—0.324, 1.540—1.564, 0.504—0.522, and 0.809—0.829 mg/mL. Conclusion This method is simple and rapid, and can be used for the quality control of XOL with satisfactory separation and repeatability.更多还原