UHPLC法同时测定苏子降气丸中10个成分含量的研究  

Simultaneous determination of ten consituents in Suzi Jiangqi pills by UHPLC

作　　者：王辉 张雁 WANG Hui;ZHANG Yan(People’s Hospital of Anji,Huzhou 313310,China;Hunan Xiangtan Institute for Food and Drug Control,Xiangtan 411100,China)

机构地区：[1]安吉县人民医院,湖州313310 [2]湖南省湘潭市食品药品检验所,湘潭411100

出　　处：《药物分析杂志》2020年第3期554-561,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立超高效液相色谱法(UHPLC法)同时测定苏子降气丸中阿魏酸、沉香四醇、甘草苷、橙皮苷、迷迭香酸、甘草酸铵、白花前胡甲素、和厚朴酚、白花前胡乙素、厚朴酚10个成分含量。方法:采用UHPLC方法,使用AQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.8μm),以乙腈-0.1%磷酸溶液为流动相,梯度洗脱,流速0.2 mL·min-1、检测波长280 nm、柱温30℃、进样量2μL。结果:阿魏酸、沉香四醇、甘草苷、橙皮苷、迷迭香酸、甘草酸铵、白花前胡甲素、厚朴酚、白花前胡乙素和厚朴酚含量测定结果分别为0.102 3~0.135 2、0.132 6~0.164 1、0.584 7~0.634 1、4.725~5.215、0.405 8~0.475 2、2.25 8~2.684、1.105~1.401、0.763 2~0.962 1、0.319 6~0.352 5、1.762~2.215 mg·g-1;线性范围分别为1.001~18.02μg·mL-1(r=0.999 8)、1.224~22.04μg·mL-1(r=0.999 6)、4.778~86.00μg·mL-1(r=0.999 4)、38.80~698.4μg·mL-1(r=0.999 7)、3.752~67.54μg·mL-1(r=0.999 5)、20.52~369.4μg·mL-1(r=0.999 5)、9.916~178.5μg·mL-1(r=0.999 4)、7.262~130.7μg·m L-1(r=0.999 8)、2.624~47.23μg·mL-1(r=0.999 5)、14.86~267.5μg·mL-1(r=0.999 4);定量下限分别为0.862、1.124、0.905、0.921、1.172、1.231、1.201、1.132、1.057、1.325μg·mL-1;平均加样回收率(n=6)分别为99.2%、98.9%、98.8%、98.6%、99.0%、98.6%、98.5%、98.8%、98.6%、98.4%(RSD<2.0%);精密度(n=6)、重复性(n=6)、稳定性(48 h)(n=7)试验的RSD<2.0%。结论:所建立的多成分测定方法快捷、准确,重复性好,可用于苏子降气丸的质量控制。Objective:To establish an UHPLC method for the simultaneous determination of 10 components in Suzi Jiangqi pills including ferulic acid,agarotetrol,liquiritin,hesperidin,rosmarinic acid,ammonium glycyrrhizinate,praeruptorin A,honokiol,praeruptorin B and magnolol. Methods:UHPLC was adopted using AQUITY UPLC BEH C18(2.1 mm ×100 mm,1.8 μm)column and the mobile phase was acetonitrile-0.1% phosphoric acid solution with gradient elution at a flow rate of 0.2 mL·min-1. The detection wavelength was 280 nm,and the column temperature was 30 ℃ and the injection volume was 2 μL. Results:Determination results of ferulic acid,agarotetrol,liquiritin,hesperidin,rosmarinic acid,ammonium glycyrrhizinate,praeruptorin A,honokiol,praeruptorin B and magnolol were 0.102 3-0.135 2 mg·g-1,0.132 6-0.164 1 mg·g-1,0.584 7-0.634 1 mg·g-1,4.725-5.215 mg·g-1,0.405 8-0.475 2 mg·g-1,2.258-2.684 mg·g-1,1.105-1.401 mg·g-1,0.763 2-0.962 1 mg·g-1,0.319 6-0.352 5 mg·g-1 and 1.762~2.215 mg·g-1,respectively. The linear ranges of 10 components were 1.001-18.02 μg·mL-1(r=0.999 8),1.224-22.04 μg·mL-1(r=0.999 6),4.778-86.00 μg·mL-1(r=0.999 4),38.80-698.4 μg·mL-1(r=0.999 7),3.752-67.54 μg·mL-1(r=0.999 5),20.52-369.4 μg·mL-1(r=0.999 5),9.916-178.5 μg·mL-1(r=0.999 4),7.262-130.7 μg·mL-1(r=0.999 8),2.624-47.23 μg·mL-1(r=0.999 5)and 14.86-267.5 μg·mL-1(r=0.999 4),respectively. Limits of quantitation were 0.862,1.124,0.905,0.921,1.172,1.231,1.201,1.132,1.057 and 1.325 μg·mL-1,respectively. The average recoveries(n=6)were 99.2%,98.9%,98.8%,98.6%,99.0%,98.6%,98.5%.,98.8%,98.6% and 98.4% respectively with RSDs all below 2.0%. RSDs of precision(n=6),reproducibility(n=6)and stability tests(48 h)(n=7)were bel ow 2.0%. Conclusion:The established multi-component method is fast,accurate and reproducible. It can be used for the quality control of Suzi Jiangqi pills.

关 键 词：苏子降气丸 阿魏酸 沉香四醇 甘草苷 橙皮苷 迷迭香酸 甘草酸铵 白花前胡甲素 和厚朴酚 白花前胡乙素 厚朴酚 超高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]