HPLC波长切换法同时测定理气散结颗粒中4个成分的含量  

Simultaneous determination of 4 components in Liqi Sanjie Keli by HPLC wavelength switching method

作　　者：李霞[1] 王毅[1] 魏谭军[1] 程阔菊[1] 

机构地区：[1]四川省达州市中西医结合医院,四川达州635000

出　　处：《实用药物与临床》2017年第2期212-215,共4页Practical Pharmacy and Clinical Remedies

基　　金：四川省科技支撑计划项目(2014SZ0189)

摘　　要：目的建立同时测定理气散结颗粒中氧化芍药苷、芍药内酯苷、芍药苷和α-香附酮的HPLC波长切换联合梯度洗脱法。方法采用Venusil MP C18色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱(0~15 min,12.0%A;15~31 min,12.0%A→26.0%A;31~39 min,26.0%A→40.0%A;39~45 min,40.0%A→12.0%A),流速0.9 mL/min,波长切换(0~31 min,在230 nm波长下检测氧化芍药苷、芍药内酯苷和芍药苷;31~45 min,在242 nm波长下检测α-香附酮),柱温30℃,进样量为20μL。结果氧化芍药苷、芍药内酯苷、芍药苷和α-香附酮4个成分的质量浓度分别在5.15~103.00μg/mL(r=0.999 6)、8.99~179.80μg/mL(r=0.999 5)、19.83~396.60μg/mL(r=0.999 9)、6.35~127.00μg/mL(r=0.999 3)呈良好线性关系;平均加样回收率及相应的RSD(n=6)分别为96.83%(0.93%)、97.85%(1.31%)、99.71%(0.80%)、98.77%(1.59%)。结论所建立的方法灵敏度高、快速、专属性好、准确度高,为理气散结颗粒的质量控制提供了依据。Objective To develop a joint gradient elution HPLC wavelength switching method for determination of the content of oxypaeoniflorin,alibiflorin,paeoniflorin and α-eyperone in Liqi Sanjie Keli simultaneously.Methods The Venusil MP C18（4.6 mm×250 mm,5 μm） chromatographic column was adopted;the mobile phase was acetonitrile（A）-0.1%phosphoric acid solution（B） with gradient elution（0~15 min,12.0%A;15~31 min,12.0%A→26.0%A;31~39 min 26.0%A→40.0%A;39~45 min,40.0%A→12.0%A）,at a flow rate of 0.9 mL/min;the detection wavelengths were set at 230 nm in 0~31 min to determine oxypaeoniflorin,alibiflorin and paeoniflorin,and 242 nm in 31~45 min to determine α-cyperone;the column temperature was set at 30 ℃;sample quantity was 20 μL.Results The quality concentration of oxypaeoniflorin,alibiflorin,paeoniflorin and α-eyperone was in good linear relationship within 5.15~103.00 μg/mL（r=0.999 6）,8.99~179.80 μg/mL（r=0.999 5）,19.83~396.60μg/mL（r = 0.999 9） and 6.35~127.00 μg/mL（r = 0.999 3） respectively.The average recoveries and the corresponding RSD were 96.83%（0.93%）,97.85%（1.31%）,99.71%（0.80%） and 98.77%（1.59%）,respectively.Conclusion The established method is highly sensitive and rapid with good specificity and high accuracy.It can be applied to the quality control of Liqi Sanjie Keli.

关 键 词：理气散结颗粒 氧化芍药苷 芍药内酯苷 芍药苷 Α-香附酮 波长切换 中成药多组分测定 

分 类 号：R286.0[医药卫生—中药学]