小儿豉翘清热颗粒HPLC-PAD指纹图谱的建立及有效成分含量测定
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摘要:
利用高效液相色谱-二极管阵列检测器(HPLC-PAD)分析检测技术,研究了提取条件(提取溶剂、提取时间)和色谱条件(洗脱溶剂、色谱柱、检测波长)的影响,最终建立了小儿豉翘清热颗粒的指纹图谱和有效成分栀子苷、连翘苷含量测定的方法.在Waters Symmtery-C18色谱柱温30℃、检测波长225nm处,以甲醇和0.1%(体积分数)的磷酸水溶液为流动相进行梯度洗脱建立的小儿豉翘清热颗粒HPLC-PAD的指纹图谱,30个色谱峰分离度良好,10批样品相似度较高(>0.98);栀子苷、连翘苷线性范围良好,相关系数(r)均大于0.999 9,相对标准偏差(Relative Standard Deviation,RSD)均小于3%,加样回收率均大于97%,RSD<3%(n=6).此方法特征性和专属性强,灵敏、准确,可作为小儿豉翘清热颗粒质量评价的方法.
The extraction conditions（extraction solvent,extraction time）and chromatographic conditions（elution solvent,chromatographic column,detection wavelength）were investigated by high performance liquid chromatography-photodiode array detector（HPLC-PAD）,it established an HPLC-PAD method for fingerprint analysis of Xiaoer Chiqiao Qingre Granules to determine the contents of geniposide and forsythin.Separation was performed using HPLC-PAD and Waters Symmtery C18 column,the gradient elution was performed by the mobile phase consisting of methanol-0.1%（volume fraction）phosphoric acid at 30 ℃ column temperature,and the detection wavelength of 225 nm,thirty peaks were selected as the specific fingerprint peaks through 10 batches Xiaoer Chiqiao Qingre Granules with the identified of geniposide and forsythin,good similarities were obtained in the established fingerprint through similarity analysis and the resolution was good,the method showed good linearity of geniposide and forsythin with correlation coefficients greater than 0.98,the correlation coefficients all greater than 0.999 9,the relative standard deviation（RSD）of precision repeatability and stability were all less than 3%,the recovery rates was all greater than 97%,and the RSD was less than 3%（n=6）.The method is specific,sensitive and accurate,and can be used for the quality control of Xiaoer Chiqiao Qingre Granules.
作者:
许文清 魏学涛 马青青 崔向前 李伟
Xu Wenqing;Wei Xuetao;Ma Qingqing;Cui Xiangqian;Li Wei(Department of public security;Department of criminal science and technology,Railway Police College,Zbengzbou 450053,Cbina;Henan Center For Disease Control and Prevention,Zbengzbou 450000,China)
机构地区:
铁道警察学院治安学系 河南省疾病预防控制中心 铁道警察学院刑事科学技术系
出处:
《betway官方app 学报：自然科学版》 CAS 北大核心 2018年第4期60-66,共7页
基金:
河南省科技攻关项目(132300410401) 河南省科技厅项目(122400450334) 铁道警察学院教学改革研究项目(JY2017028)
关键词:
小儿豉翘清热颗粒 HPLC-PAD 指纹图谱 含量测定
Xiaocr Chiqiao Qingre Granules HPLC PAD fingerprint determination of components
分类号:
R286.0 [医药卫生—中药学] O657.72 [理学—分析化学]
