提取黑果腺肋花楸果中金丝桃苷的工艺
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摘要
建立黑果腺肋花楸果中金丝桃苷的含量测定方法,并优化离子液体超声辅助提取金丝桃苷的工艺条件。以金丝桃苷的提取率为指标,采用高效液相色谱法测定黑果腺肋花楸果中金丝桃苷的含量,色谱柱采用伊利特ODS2 C_(18) (4.6 mm×250 mm, 5μm),流动相以乙腈-0.25%醋酸水溶液梯度洗脱,进样量20μL,检测波长360 nm,柱温30℃。在建立含量测定方法的同时探索离子液体超声辅助提取黑果腺肋花楸果中金丝桃苷的工艺条件。结果表明,金丝桃苷在0.97～18.40μg·mL~(-1)浓度范围内线性关系良好(r=0.998 1),平均回收率为98.17%, RSD为1.89%;金丝桃苷的最佳提取工艺:离子液体为1-丁基-3-甲基咪唑硝酸盐,其浓度为0.05 mol·L-1,料液比为1︰25 (g/mL),乙醇体积分数为60%,提取温度为70～80℃,提取时间为35 min,超声波功率为80 W。在优化提取条件下,金丝桃苷的提取率为27.37μg·g~(-1)。该含量测定方法精密度良好,结果准确可靠;优化的提取方法快速、简单、提取率高,为黑果腺肋花楸果的开发利用提供了依据。
To establish a method for the determination of hyperin in the fruit of Aronia melanocarpa, and to optimize the technological conditions of ultrasonic-assisted extraction of hyperin from ionic liquid, taking the extraction rate of hyperoside as an index, the content of hyperin in the fruit of Aroni amelanocarpa was determined by high performance liquid chromatography(HPLC). The chromatographic separation was performed in Illiot ODS2 colum(C18, 4.6 mm×250 mm, 5 μm). The mobile phase was eluted with a gradient of acetonitrile-0.25% acetic acid. The injection volume was 20 μL, the detection wavelength was 360 nm, and the column temperature was 30 ℃. The technological conditions of ultrasonic extraction of hyperin in the fruit of Aronia melanocarpa were explored, when a method of determination was established. The test results showed that the good linear relationship of hyperin was 0.97-18.40 μg·mL-1(r=0.998 1), its average recovery was 98.17%, and RSD was 1.89%. The best extraction process of hyperin was that ionic liquid was 1-butyl-3-methylimidazolium nitrate, its concentration was 0.05 mol·L-1, the ratio of material and liquid was 1︰25(g/m L), the volume fraction of ethanol was 60%, the extraction temperature was 70-80 ℃, the extraction time was 35 min, and the ultrasonic power was 80 W. The extraction yield of hyperin was 27.37 μg·g-1 under optimized extraction conditions. The method of determination had good precision, and the result was accurate and reliable. The optimized extraction method was fast and simple, and the extraction rate was high, which provided the basis for the development and utilization of the Aroni amelanocarpa.
To establish a method for the determination of hyperin in the fruit of Aronia melanocarpa, and to optimize the technological conditions of ultrasonic-assisted extraction of hyperin from ionic liquid, taking the extraction rate of hyperoside as an index, the content of hyperin in the fruit of Aroni amelanocarpa was determined by high performance liquid chromatography(HPLC). The chromatographic separation was performed in Illiot ODS2 colum(C18, 4.6 mm×250 mm, 5 μm). The mobile phase was eluted with a gradient of acetonitrile-0.25% acetic acid. The injection volume was 20 μL, the detection wavelength was 360 nm, and the column temperature was 30 ℃. The technological conditions of ultrasonic extraction of hyperin in the fruit of Aronia melanocarpa were explored, when a method of determination was established. The test results showed that the good linear relationship of hyperin was 0.97-18.40 μg·mL-1(r=0.998 1), its average recovery was 98.17%, and RSD was 1.89%. The best extraction process of hyperin was that ionic liquid was 1-butyl-3-methylimidazolium nitrate, its concentration was 0.05 mol·L-1, the ratio of material and liquid was 1︰25(g/m L), the volume fraction of ethanol was 60%, the extraction temperature was 70-80 ℃, the extraction time was 35 min, and the ultrasonic power was 80 W. The extraction yield of hyperin was 27.37 μg·g-1 under optimized extraction conditions. The method of determination had good precision, and the result was accurate and reliable. The optimized extraction method was fast and simple, and the extraction rate was high, which provided the basis for the development and utilization of the Aroni amelanocarpa.
引文
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[17]王志兵,张洪玉,薛瑾,等.超声辅助均相离子液体微萃取-高效液相色谱法测定丹参中的丹参酮[J].现代食品科技,2015,31(4):294-299.
[18]王珍,李秀霞,李娇,等.高效液相色谱法测定山楂中芦丁、金丝桃苷和槲皮素的含量[J].食品工业科技,2013,34(9):302-305.
[19]刘翔宇,赵培,阎亚丽,等.小扁豆中多酚物质的提取与组分鉴定[J].食品与机械,2016,32(3):154-159.
[20]王顺新,牟德华,王小伟.超声波辅助提取人参果叶黄酮工艺研究[J].食品工业,2016,37(5):68-70.
[21]魏金凤,张志娟,李冬冬,等.离子液体辅助萃取山高粱中4种黄酮类成分的研究[J].中国中药杂志,2015,40(7):1305-1309.
[22]陈君,周光明,杨远高,等.离子液体-超声辅助萃取/高效液相色谱法测定白花杜鹃叶中的黄酮[J].分析测试学报,2013,32(3):341-345.
[2]杨苑艺,李晶莹,吴佳琳,等.黑果花楸果实多酚提取工艺的研究[J].森林工程,2015,31(5):24-29.
[3]吐尔尼沙·吐尔逊,马旦·山泰.黑果花楸开发利用价值及繁殖方法探析[J].园艺与种苗,2015(8):11-12.
[4]KULLING S E,RAWEL H M.Chokeberry(Aronia melanocarpa)-A review on the characteristic componentsand potential health effects[J].Planta Med,2008,74(10):1625-1634.
[5]OSZMIA SKI J,WOJDYLO A.Aronia melanocarpa phenolics and their antioxidant activity[J].Europe Food Res Technol,2005,221(8):809-813.
[6]HANDELAND M,GRUDE N,TORP T,et al.Black chokeberry juice(Aronia melanocarpa)reduces incidences of urinary tract infection among nursing home residents in the long term-A pilot study[J].Nutrition Research,2014,34(6):518-525.
[7]BADESCU M,BADULESCU O,BADESCU L,et al.Effects of Sambucus nigra and Aronia melanocarpa extracts on immune system disorders within diabetes mellitus[J].Pharmaceutical Biology,2015,53(4):533-539.
[8]张衡锋,韦庆翠,汤庚国,等.不同基质配比对黑果腺肋花楸容器苗生长及叶片生理特性的影响[J].北方园艺,2017(20):104-109.
[9]李根柱,张自川.黑果腺肋花楸苗木扦插繁殖研究[J].北方园艺,2016(17):37-39.
[10]于明.黑果腺肋花楸和头花蓼的化学成分及其生物活性的研究[D].沈阳:沈阳药科大学,2006.
[11]侯秋苑,冯白茹,申茹,等.菟丝子中金丝桃苷的提取工艺优选[J].汕头大学医学院学报,2017,30(3):141-142,159.
[12]玄永浩,金英善.黑果腺肋花楸化学成分及药理活性研究进展[J].现代农业科技,2009(20):101-102,104.
[13]贲永光,苏健裕,杨鼎隆.基于离子液体超声辅助提取菊花绿原酸的试验研究[J].中国食品学报,2014,14(10):164-169.
[14]陈明明,赵思敏,王毅帆,等.离子液体辅助超声提取黄柏总生物碱[J].沈阳药科大学学报,2015,32(11):859-863.
[15]XIAO Y,WANG Y,GAO S Q,et al.Determination of the active constituents in Arnebia euchroma(Royle)Johnst by ionic liquid-based ultrasonic-assisted extraction highperformance liquid chromatography[J].Journal of Chromatography B,2011,879(20):1833-1838.
[16]史丽娟,彭胜,郑阳,等.离子液体超声波辅助法提取杜仲皮总木脂素的工艺研究[J].应用化工,2015,44(12):2250-2254.
[17]王志兵,张洪玉,薛瑾,等.超声辅助均相离子液体微萃取-高效液相色谱法测定丹参中的丹参酮[J].现代食品科技,2015,31(4):294-299.
[18]王珍,李秀霞,李娇,等.高效液相色谱法测定山楂中芦丁、金丝桃苷和槲皮素的含量[J].食品工业科技,2013,34(9):302-305.
[19]刘翔宇,赵培,阎亚丽,等.小扁豆中多酚物质的提取与组分鉴定[J].食品与机械,2016,32(3):154-159.
[20]王顺新,牟德华,王小伟.超声波辅助提取人参果叶黄酮工艺研究[J].食品工业,2016,37(5):68-70.
[21]魏金凤,张志娟,李冬冬,等.离子液体辅助萃取山高粱中4种黄酮类成分的研究[J].中国中药杂志,2015,40(7):1305-1309.
[22]陈君,周光明,杨远高,等.离子液体-超声辅助萃取/高效液相色谱法测定白花杜鹃叶中的黄酮[J].分析测试学报,2013,32(3):341-345.