HPLC-MS/MS法同时测定橘茴排石颗粒中13种成分的含量  

Simultaneous Determination of 13 Components in Juhuipaishi Granules by HPLC-MS/MS

作　　者：徐小龙 王榆翔 王斌[1] Xu Xiaolong;Wang Yuxiang;Wang Bin(Department of Pharmacy,Lianyungang Hospital of Traditional Chinese Medicine Affiliated to Nanjing University of Chinese Medicine,Lianyungang 222000,China)

机构地区：[1]江苏省连云港市中医院药学部南京中医药大学连云港附属医院,江苏连云港222000

出　　处：《广东化工》2025年第6期138-140,共3页Guangdong Chemical Industry

基　　金：连云港市卫生科技项目(QN202205);2022年度连云港市中医药科技发展计划项目(YB202203);南京医科大学康达学院2024年度科研发展基金课题(KD2024KYJJ085);江苏省药学会—奥赛康医院药学科研基金课题(A202435)。

摘　　要：目的:建立液质联用法对橘茴排石颗粒中13种化学成分:绿原酸、槲皮素、黄芩苷、没食子酸、香豆素、桂皮酸、桂皮醛、辛弗林、原儿茶醛、羟甲香豆素、咖啡酸、芦丁、柚皮苷有效识别和定量分析。方法:采用液质Agilent 1290-6470LC/TQ三重四级杆液质联用仪,色谱柱:HPLC PACKED C18150×2.1 mm×2.7μm;流动相:甲醇-0.1%甲酸水溶液梯度洗脱;采用正离子和负离子模式同时监测,正离子和负离子监测模式下源喷射电压分别为5.5 kV和-4.5 kV,离子源温度为650℃,雾化气(Gas1)300 kPa,加热气(Gas2)310 kPa,接口持续加热,帘气172 kPa,全程氮气通入状态。结果:在18 min内橘茴排石颗粒中13种有效组分绿原酸、槲皮素、黄芩苷、没食子酸、香豆素、桂皮酸、桂皮醛、辛弗林、原儿茶醛、羟甲香豆素、咖啡酸、芦丁、柚皮苷被分离并能有效化学识别和定量分析。结果:液质联用法能简单快捷识别橘茴排石颗粒特征成分并对其定量分析,各组分峰面积与其浓度呈良好的线性;平均回收率范围为89.2%~115.3%,RSD为0.86%~3.26%。结论:本文建立的方法经验证简便、重现性好、专属性高,可为橘茴排石颗粒质量控制提供参考。Objective:To establish an effective liquid chromatography-mass spectrometry(LC-MS)for the identification and quantitative analysis of 13 chemicacomponents in orange fennite granules:chlorogenic acid,quercetin,baicalin,gallic acid,coumarin,cinnamic acid,cinnamaldehyde,synephrine,protocatechin,oxymethylcoumarin,caffeic acid,rutin,and naringin.Methods:Liquid Agilent 1290-6470LC/TQ triple quadrupole LC/MS column:HPLC PACKED C18150×2.1 mm×2.7μm;Mobile phase:methanol-0.1%formic acid aqueous solution gradient elution;The source injection voltage is 5.5 kV and-4.5 kV respectively,the ion source temperature is 650℃,the atomized gas(Gas1)is 300 kPa,the heating gas(Gas2)is 310 kPa,the interface is continuously heated,the curtain gas is 172 kPa,and the nitrogen is in the state of the whole process.Results Chlorogenic acid,quercetin,baicalin,gallic acid,coumarin,cinnamic acid,cinnamal acid,cinnamaldehyde,synephrine,protocatehydehyde,oxymethylcoumarin,caffeic acid,rutin,naringin were isolated and effectively chemically identified and quantified in 18 min.Results:Liquid chromatography-mass spectrometry(LC-MS)could easily and quickly identify the characteristic components of orange anise stone particles and analyze them quantitatively,and the peak area and concentration of each component showed good linearity.The average recoveries ranged from 89.2%~115.3%and the RSD ranged from 0.86%~3.26%.Conclusion:The method established in this paper is simple,reproducible and specific,which can provide a reference for the quality control of orange fennite particles.

关 键 词：医院制剂 橘茴排石颗粒 化学识别 高效液相色谱-质谱联用法 

分 类 号：R9[医药卫生—药学]