粗壮女贞功效成分的含量测定和超声提取工艺  

Content Determination and Ultrasonic-assistant Extraction Technology of the Functional Compositions in Ligustrum robustum

作　　者：梁小娜 陈雪 韦红宇 吴青 陆世惠 LIANG Xiaona;CHEN Xue;WEI Hongyu;WU Qing;LU Shihui(College of Pharmacy,Youjiang Medical University for Nationalities,Baise 533000,China;Guangxi Database Construction and Application Engineering Research Center for in Tracorporal Pharmacochemistry of TCM,Baise 533000,China;Key Laboratory of Youjiang Basin Characteristic Ethnic Medicine Research in Guangxi,Baise 533000,China)

机构地区：[1]右江民族医学院药学院,百色533000 [2]广西壮族自治区中药体内药物化学数据库建设与应用工程研究中心,百色533000 [3]广西高校右江流域特色民族药研究重点实验室,百色533000

出　　处：《医药导报》2025年第1期96-102,共7页Herald of Medicine

基　　金：广西科技基地和人才专项项目(桂科AD21075006);广西自然科学基金面上项目(2020GXNSFAA-297129)。

摘　　要：目的建立紫外分光光度法(UV)测定粗壮女贞功效成分(肉桂酸衍生物、总黄酮)含量,并基于UV/高效液相色谱(HPLC)预测其中的反式对羟基肉桂酸及其酯、野漆树苷的含量,同时优化其超声提取工艺条件。方法①在粗壮女贞功效成分的含量测定中,用双波长等吸收点UV法(检测波长316 nm,参比波长268 nm)测定肉桂酸衍生物总含量,单波长UV法(检测波长268 nm)测定总黄酮含量,HPLC法(C 18色谱柱,甲醇-0.1%醋酸溶液=40:60洗脱,检测波长310 nm)测定野漆树苷等的含量;②用转换因子建立基于UV/HPLC的预测模型,并以另外3个测试样本检验预测结果的准确性;③用正交实验法优化超声提取工艺条件。结果①肉桂酸衍生物、总黄酮、野漆树苷的线性范围分别为4.64~20.88、8.24~28.84、5.15~51.50μg·mL^(-1)(r≥0.9995),精密度、稳定性、重复性实验的相对标准偏差(RSD)≤1.4%,加样回收率97.9%~100.5%(RSD≤1.2%,n=6);②UV/HPLC预测值与HPLC实测值相对误差-5.3%~1.7%,反式对羟基肉桂酸、野漆树苷含量的预测值与实测值差异无统计学意义(P>0.05);③超声提取粗壮女贞的最佳工艺条件为乙醇浓度80%、温度50℃、液料比20 mL·g^(-1)、提取2次、提取20 min,在该条件下功效成分总产率为42.0%。结论建立的含量测定方法准确、快速,提取方法高效、节能、省时,为粗壮女贞的质量控制和开发利用提供了实验依据。Objective To establish a UV method for the determination of the functional compositions(cinnamic acid derivatives,total flavonoids)in Ligustrum robustum,to predict the contents of trans-p-hydroxycinnamic acid,trans-p-hydroxycinnamic acid esters,and rhoifolin based on UV/HPLC,and to optimize the technological conditions of ultrasonic-assistant extraction of L.robustum.Methods①In the determination of the functional compositions in L.robustum,total cinnamic acid derivatives were determined by dual-wavelength isobestic point UV method(detection wavelength 316 nm,reference wavelength 268 nm),and total flavonoids were determined by single-wavelength UV method(detection wavelength 268 nm),while rhoifolin was determined by HPLC(C 18 column,eluting with methanol-0.1%acetic acid=40:60,detection wavelength 310 nm).②The conversion factors were used to establish a UV/HPLC-based prediction model,and the precision of the predicted results was evaluated with other 3 test samples.③The technological conditions of ultrasonic-assisted extraction were optimized by an orthogonal test.Results①The linear ranges of total cinnamic acid derivatives,total flavonoids,and rhoifolin were 4.64-20.88,8.24-28.84,5.15-51.50μg·mL^(-1)(r≥0.9995),respectively.RSDs of the precision,stability,and reproducibility tests were no more than 1.4%.The recoveries were 97.9%-100.5%(RSD≤1.2%,n=6).②The relative errors of the values predicted by UV/HPLC from the results measured by HPLC were from-5.3%to 1.7%.There was no significant difference between the UV/HPLC predicted values and the HPLC determined results(P>0.05)for the contents of trans-p-hydroxycinnamic acid and rhoifolin.③The optimal technological conditions of ultrasonic-assistant extraction of L.robustum were as follows:ethanol concentration 80%,temperature 50℃,liquid-solid ratio 20 mL·g^(-1),extraction frequency 2 times,extraction time 20 min.The total yield of functional compositions under above conditions was 42.0%.Conclusion The above determination methods are accurate and rapid

关 键 词：粗壮女贞 功效成分 含量测定 提取工艺 

分 类 号：R282.71[医药卫生—中药学] R284.2[医药卫生—中医学]