大戟脂药材中四环三萜类成分大戟二烯醇、大戟醇的含量测定及提取工艺优化  

Content Determination of Tetracyclic Triterpenoids as Euphol and Euphorbol in Euphorbium resinifera and the Optimization of Extraction Technology

作　　者：刘婧 李晨阳 赵军 顾政一 LIU Jing;LI Chenyang;ZHAO Jun;GU Zhengyi(School of Pharmacy,Shihezi University,Xinjiang Shihezi 832000,China;Key Laboratory of Uyghur Medicine,Xinjiang Institute of Materia Medica,Urumqi 830004,China)

机构地区：[1]石河子大学药学院,新疆石河子832000 [2]新疆药物研究所维吾尔药重点实验室,乌鲁木齐830004

出　　处：《中国药房》2021年第6期708-712,共5页China Pharmacy

基　　金：国家重大新药创制科技重大专项。

摘　　要：目的:建立同时测定大戟脂药材中大戟二烯醇和大戟醇含量的方法,并优化其提取工艺。方法:采用高效液相色谱法。色谱柱为Agilent ZORBAX Eclipse Plus C8,流动相为乙腈-水(90∶10,V/V),流速为1.0 mL/min,检测波长为210 nm,柱温为30℃,进样量为10μL。以大戟二烯醇、大戟醇含量、出膏率为评价指标进行综合评分,以乙醇体积分数、提取时间、溶剂用量为考察因素,采用L9(34)正交试验优化其提取工艺并进行验证。结果:大戟二烯醇、大戟醇检测质量浓度的线性范围分别为0.0304~1.216mg/mL(r=0.9996)、0.01~0.4 mg/mL(r=0.9999);精密度、稳定性(24 h)、重复性试验的RSD均小于2%,平均加样回收率分别为100.46%(RSD=1.03%,n=6)、99.36%(RSD=0.91%,n=6)。最优提取工艺为40 mL的95%乙醇回流提取1 h。经3次试验验证结果显示,大戟二烯醇的平均含量为94.43 mg/g(RSD=0.92%,n=3),大戟醇的平均含量为25.42 mg/g(RSD=0.98%,n=3),平均出膏率为51.42%,(RSD=1.95%,n=3),平均综合评分为98.87(RSD=0.92%,n=3)。结论:所建含量测定方法简便、准确,重复性好,可用于大戟脂的质量控制;优化所得提取工艺稳定、可行。OBJECTIVE:To establish a method for the simultaneous determination of euphol and euphorbol in Euphorbium resinifera,and to optimize the extraction technology.METHODS:HPLC method was adopted.The determination was performed on Agilent ZORBAX Eclipse Plus C8 column with mobile phase consisted of acetonitrile-water(90∶10,V/V)at the flow rate of 1.0 mL/min.The detection wavelength was set at 210 nm,and column temperature was 30℃.The sample size was 10μL.Using the contents of euphol and euphorbol,yield of the extract as evaluation index,comprehensive score was conducted.The extraction technology was optimized by L9(34)orthogonal tests,with ethanol volume fraction,extraction time and solvent dosage as factors.RESULTS:The linear ranges of euphol and euphorbol were 0.0304-1.216 mg/mL(r=0.9996)and 0.01-0.4 mg/mL(r=0.9999),respectively.RSDs of precision,stability(24 h)and producibility tests were all lower than 2%.Average recoveries were 100.46%(RSD=1.03%,n=6)and 99.36%(RSD=0.91%,n=6).The optimized technology was extracting with 40 mL 95%ethanol for 1 h.After 3 times of validation tests showed that average content of euphol was 94.43 mg/g(RSD=0.92%,n=3),and that of euphorbol was 25.42 mg/g(RSD=0.98%,n=3);average yield of the extract was 51.42%(RSD=1.95%,n=3),and average comprehensive score was 98.87(RSD=0.92%,n=3).CONCLUSIONS:Established method is simple,accurate and reproducible,which can be used for the quality control of E.resinifera.The optimized extraction technology is simple and stable.

关 键 词：大戟脂 大戟二烯醇 大戟醇 高效液相色谱法 含量测定 提取工艺优化 

分 类 号：R284.2[医药卫生—中药学]