UPLC法同时测定痛泻要方及其破壁饮片中7种活性成分的含量  

Simultaneous Determination of Seven Active Components in Tongxie Yaofang Formula and Ultrafine Granular Powder by Ultra-performance Liquid Chromatography

作　　者：胡莹[1] 郑依玲 梅全喜[1] 董鹏鹏 高玉桥[1] 钟希文[1] 曾聪彦[1] 胡玉良[1] 

机构地区：[1]中山市中医院,广东中山528400

出　　处：《中药新药与临床药理》2017年第6期786-791,共6页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：中山市科技局科研课题(2016B1046)

摘　　要：目的建立超高效液相色谱(UPLC)法同时测定痛泻要方(TXYF)及其破壁饮片中芍药内酯苷、芍药苷、升麻素、芸香柚皮苷、5-O-甲基维斯阿米醇苷、橙皮苷、川陈皮素7种成分的含量,为痛泻要方破壁饮片的质量控制提供依据。方法以UPLC法,色谱柱为Waters Acquity UPLC BEH C_(18)(100 mm×2.1 mm,1.7μm)为色谱柱,采用乙腈-0.1%甲酸为流动相,梯度洗脱;流速:0.3 m L·min^(-1);检测波长为240 nm;柱温35℃;进样量2μL。测定痛泻要方饮片及破壁饮片中芍药内酯苷、芍药苷、升麻素、芸香柚皮苷、5-O-甲基维斯阿米醇苷、橙皮苷、川陈皮素7种成分的含量。结果芍药内酯苷、芍药苷、升麻素、芸香柚皮苷、5-O-甲基维斯阿米醇苷、橙皮苷、川陈皮素分别在0.031 4~1.006μg(r=0.999 8),0.103 8~3.32μg(r=0.999 8),0.007 8~0.248μg(r=0.999 4),0.02~0.64μg(r=0.999 9),0.013 4~0.43μg(r=1),0.012 7~0.407μg(r=0.999 8),0.000 5~0.015 5μg(r=0.999 8)浓度范围内呈现良好的线性关系;平均回收率:痛泻要方饮片分别为99.67%、99.68%、99.75%、99.70%、99.19%、99.92%、99.85%;痛泻要方破壁饮片分别为99.41%、100.06%、99.62%、99.92%、99.77%、99.97%、99.91%(n=9)。结论该方法简便、快速、精确、重复性良好,结果准确可靠,可用于痛泻要方饮片及破壁饮片的质量控制。Objective The aim of this study was to establish a method for the simultaneous determination of albiflorin,paeoniflorin, cimifugin, narirutin, hesperidin, 4＇-O-β-D-glucosyl-5-O-methylvismminol, nobiletin in Tongxie Yaofang（TXYF） herb formula and ultrafine granular powder,to apply as the quality control method of the herb and ultrafine granular powder. Methods A separation was achieved using Waters Acquity UPLC BEH C_（18） column（100 mm×2.1 mm,1.7 μm） with a gradient elution program consisting of acetonitrile and 0.1 % formic acid solution at a flow rate of 0.3 m L·min-1. The detection wavelength was set at 240 nm. The column temperature was 35 ℃,and the injection volume was 2 μL. The method was validated for specificity, linearity, accuracy, precision, limit of detection, and limit of quantification. Results The linear range was 0.031 4-1.006 μg（r=0.999 8） for albiflorin,0.103 8-3.32 μg（r=0.999 8）for paeoniflorin,0.007 8-0.248 μg（r=0.999 4）for cimifugin,0.02-0.64 μg（r=0.999 9）for narirutin,0.013 4-0.43 μg（r=1）for hesperidin,0.012 7-0.407 μg（r=0.999 8）for 4＇-O-β-D-glucosyl-5-Omethylvismminol,0.000 5-0.015 5 μg（r=0.999 8） for nobiletin. The average recoveries（n=9） of seven components herb pieces were 99.67 %,99.68 %,99.75 %,99.70 %,99.19 %,99.92 % and 99.85 %;for ultrafine granular powder the seven herbs were 99.41 %, 100.06 %, 99.62 %, 99.92 %, 99.77 %, 99.97% and 99.91 %,respectively. Conclusion The established method is simple, rapid, accurate and reproducible. The results were accurate and reliable. It can be used for the quality control of herb and ultrafine granular powder of TXYF formula.

关 键 词：痛泻要方 活性成分 破壁饮片 质量控制 超高效液相色谱 

分 类 号：R284.1[医药卫生—中药学]