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粗壮女贞功效成分的含量测定和超声提取工艺

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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(C18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、5.15~51.50 μg·mL-1(r≥0.999 5),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.
Content Determination and Ultrasonic-assistant Extraction Technology of the Functional Compositions in Ligustrum robustum
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.Methods ①In 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.③ The technological conditions of ultrasonic-assisted extraction were optimized by an orthogonal test.Results ① The linear ranges of total cinnamic acid derivatives,total flavonoids,and rhoifolin were 4.64-20.88,8.24-28.84,5.15-51.50 μg·mL-1(r≥0.999 5),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,and the above extraction technology is effective,energy-saving and rapid,which provide an experimental base for the quality control and application of L.robustum.

Ligustrum robustumFunctional compositionDeterminationExtraction technology

梁小娜、陈雪、韦红宇、吴青、陆世惠

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右江民族医学院药学院,百色 533000

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

广西高校右江流域特色民族药研究重点实验室,百色 533000

粗壮女贞 功效成分 含量测定 提取工艺

2025

医药导报
中国药理学会 华中科技大学同济医学院附属同济医院 中国医药商业协会

医药导报

北大核心
影响因子:1.042
ISSN:1004-0781
年,卷(期):2025.44(1)