水石榴中总黄酮的提取工艺优化(1)
中图分类号 R284.2 文献标志码 A 文章编号 1001-0408(2019)20-2807-06
DOI 10.6039/j.issn.1001-0408.2019.20.14
摘 要 目的：建立水石榴中总黄酮的含量测定方法，并优化其提取工艺。方法：以三氯化铝为显色剂，采用紫外-可见光分光光度法测定水石榴中总黄酮的含量。在单因素试验的基础上，以乙醇体积分数、料液比、提取时间、提取温度、提取次数为考察因素，以水石榴中总黄酮含量为指标，采用Plackett-Burman试验筛选对总黄酮含量有显著影响的因素，利用最陡爬坡试验确定最佳取值范围，再结合Box-Behnken响应面法优化总黄酮的提取工艺。结果：总黄酮的检测质量浓度线性范围为0.012～0.036 mg/mL(r=0.999 9);精密度、稳定性、重复性试验的RSD均小于3%;加样回收率为92.98%～99.86%(RSD=2.71%，n=6)。优化所得提取工藝为乙醇体积分数60%，料液比1 ∶ 34(g/mL)，提取次数3次，提取时间60 min，提取温度80 ℃;在此工艺条件下，水石榴中总黄酮的平均含量为2.71%(RSD=1.69%，n=6)，与模型预测值(2.64%)的相对误差为2.65%。结论：所建含量测定方法稳定性、重复性均较好，可用于测定水石榴中总黄酮的含量;优化所得提取工艺稳定、可行。
关键词 水石榴;总黄酮;提取工艺;Plackett-Burman试验;Box-Behnken响应面法;紫外-可见光分光光度法;含量测定
ABSTRACT OBJECTIVE： To establish the method for content determination of total flavonoids from Combretum alfrdii， and to optimize the extraction technology of total flavonoids from C. alfrdii. METHODS： Using aluminium trichloride as， chromogenic agent， UV spectrum was adopted to determine the content of total flavonoids from C. alfrdii. Based on single factor test， ethanol volume fraction， material-liquid ratio， extraction time， extraction temperature and times were selected as investigation factors， and the content of total flavonoids was selected as response value， Plackett-Burman design was used to screen the factors that had significant influence on the content of total flavonoidsfrom C. alfrdii. Then steepest climbing test was adopted to confirm the optimum valuing range; the extraction technology of total flavonoids was optimized by Box-Behnken response methodology. RESULTS： The linear range of total flavonoids were 0.012-0.036 mg/mL (r=0.999 9); RSDs of precision， stability and repeatability tests were less than 3%; the recovery ranged from 92.98% to 99.86% (RSD=2.71%， n=6). The optimal extraction technology included that 60% ethanol， material-liquid ratio of 1 ∶ 34 (g/mL)， extracting for 3 times， lasting for 60 min， extraction temperature of 80 ℃. Under this technology， average content of total flavonoids from C. alfrdii was 2.71% (RSD=1.69%， n=6)， and the relative error was 2.65% compared with predicted value of the model (2.64%). CONCLUSIONS： Established method is stable and reproducible， and can be used for content determination of total flavonoids from C. alfrdii. The optimized extraction method is stable and feasible.
KEYWORDS Combretum alfrdii; Total flavonoids; Extraction technology; Plackett-Burman experiment; Box-Behnken response surface methodology; UV spectrophotometry; Content determination, 百拇医药(李金洲 陈勇 陈子隽 吕培群 林玉港 卢慧敏 黄艳茹)
DOI 10.6039/j.issn.1001-0408.2019.20.14
摘 要 目的：建立水石榴中总黄酮的含量测定方法，并优化其提取工艺。方法：以三氯化铝为显色剂，采用紫外-可见光分光光度法测定水石榴中总黄酮的含量。在单因素试验的基础上，以乙醇体积分数、料液比、提取时间、提取温度、提取次数为考察因素，以水石榴中总黄酮含量为指标，采用Plackett-Burman试验筛选对总黄酮含量有显著影响的因素，利用最陡爬坡试验确定最佳取值范围，再结合Box-Behnken响应面法优化总黄酮的提取工艺。结果：总黄酮的检测质量浓度线性范围为0.012～0.036 mg/mL(r=0.999 9);精密度、稳定性、重复性试验的RSD均小于3%;加样回收率为92.98%～99.86%(RSD=2.71%，n=6)。优化所得提取工藝为乙醇体积分数60%，料液比1 ∶ 34(g/mL)，提取次数3次，提取时间60 min，提取温度80 ℃;在此工艺条件下，水石榴中总黄酮的平均含量为2.71%(RSD=1.69%，n=6)，与模型预测值(2.64%)的相对误差为2.65%。结论：所建含量测定方法稳定性、重复性均较好，可用于测定水石榴中总黄酮的含量;优化所得提取工艺稳定、可行。
关键词 水石榴;总黄酮;提取工艺;Plackett-Burman试验;Box-Behnken响应面法;紫外-可见光分光光度法;含量测定
ABSTRACT OBJECTIVE： To establish the method for content determination of total flavonoids from Combretum alfrdii， and to optimize the extraction technology of total flavonoids from C. alfrdii. METHODS： Using aluminium trichloride as， chromogenic agent， UV spectrum was adopted to determine the content of total flavonoids from C. alfrdii. Based on single factor test， ethanol volume fraction， material-liquid ratio， extraction time， extraction temperature and times were selected as investigation factors， and the content of total flavonoids was selected as response value， Plackett-Burman design was used to screen the factors that had significant influence on the content of total flavonoidsfrom C. alfrdii. Then steepest climbing test was adopted to confirm the optimum valuing range; the extraction technology of total flavonoids was optimized by Box-Behnken response methodology. RESULTS： The linear range of total flavonoids were 0.012-0.036 mg/mL (r=0.999 9); RSDs of precision， stability and repeatability tests were less than 3%; the recovery ranged from 92.98% to 99.86% (RSD=2.71%， n=6). The optimal extraction technology included that 60% ethanol， material-liquid ratio of 1 ∶ 34 (g/mL)， extracting for 3 times， lasting for 60 min， extraction temperature of 80 ℃. Under this technology， average content of total flavonoids from C. alfrdii was 2.71% (RSD=1.69%， n=6)， and the relative error was 2.65% compared with predicted value of the model (2.64%). CONCLUSIONS： Established method is stable and reproducible， and can be used for content determination of total flavonoids from C. alfrdii. The optimized extraction method is stable and feasible.
KEYWORDS Combretum alfrdii; Total flavonoids; Extraction technology; Plackett-Burman experiment; Box-Behnken response surface methodology; UV spectrophotometry; Content determination, 百拇医药(李金洲 陈勇 陈子隽 吕培群 林玉港 卢慧敏 黄艳茹)
参见：首页 > 中医药 > 中医药保健 > 食疗药膳 > 食物大全 > 果品类 > 安石榴(石榴)