固相萃取-高效液相色谱法测定妇乐颗粒中大黄素、大黄酸、绿原酸和没食子酸的含量  

Determination of emodin,rhubarb acid,chlorogenic acid and gallic acid in fule granules by solid phase extraction purification combined with HPLC

作　　者：王春燕 郭鑫 陈艳梅 李丽华 李伟 WANG Chunyan;GUO Xin;CHEN Yanmei;LI Lihua;LI Wei(Department of Pharmacy,Urumqi Maternal and Child Health Hospital,Urumqi,830000,China)

机构地区：[1]乌鲁木齐市妇幼保健院药剂科,新疆维吾尔自治区乌鲁木齐830000

出　　处：《安徽医药》2023年第5期907-910,共4页Anhui Medical and Pharmaceutical Journal

摘　　要：目的 建立了固相萃取-高效液相色谱法测定妇乐颗粒中大黄素、大黄酸、绿原酸和没食子酸的含量,从洗脱溶剂的种类与体积、流动相的组成等条件优化检测方法。方法 采用HLB萃取小柱净化,3 mL的乙腈-乙酸(95∶5)作为洗脱溶剂;Thermo C_(18)柱(150 mm×4.6 mm,5μm)进行分离,流动相为质量分数为0.1%磷酸水溶液(A)-乙腈(B)梯度洗脱,洗脱程序如下:0~1 min,30%B;1~3 min,70%B;3~6 min,70%B;6~8 min,30%B;流速为1.0 mL/min,检测波长为254 nm(大黄酸和大黄素)、270 nm(没食子酸)、325 nm (绿原酸),柱温为25℃,进样量为20μL。结果 在最优的萃取条件下所建立的方法定量限为5~20 mg/L,日内、日间精密度均小于5.2%,加样回收率为95.07%~98.74%,RSD值小于5.3%。结论 该方法准确、灵敏和重复性好,为完善妇乐颗粒质量控制体系提供理论基础和实用依据。Objective To establish a solid phase extraction method-high performance liquid chromatographic analysis for the determination of emodin,rhein,gallic acid and chlorogenic acid from fule granules samples,and to optimize the detection method from the types and volumes of elution solvents and the composition of mobile phases.Methods The HLB extraction cartridge was used for purification with 3 mL of acetonitrile acetic acid(95∶5) as elution solution.The Thermo C_(18) column(150 mm×4.6 mm,5 μm) was used to separation.The mobile phase was gradient elution of 0.1% phosphoric acid solution(A)/acetonitrile(B).The elution procedure was as follows:0-1 min,30% B;1-3 min,70% B;3-6 min,70% B;6-8 min,30% B.The flow rate was 1.0 mL/min,the detection wavelengths were set at 254 nm(emodin and rhein),270 nm(gallic acid) and 325 nm(chlorogenic acid).Column temperature was 25 ℃ with 20 μL of injection volume.Results Under the optimal extraction condition,the quantitative limit of the method was 5-20 mg/L,and the intraday and interday precision was less than 5.2%,the recovery rate was 95.07%-98.74% with RSD5.3%.Conclution The developed method is accurate,sensitive and reproducible,which provides theoretical basis and practical introduction for improving the quality control system of fule granules.

关 键 词：主成分分析 固相萃取 高效液相色谱 妇乐颗粒 

分 类 号：O657.72[理学—分析化学] R286.0[理学—化学]