星点设计优化野黄芩素制备工艺
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摘要
采用星点设计法(Central composite design,CCD)优化灯盏乙素水解制备野黄芩素的反应条件。选取反应温度及介质固液比为主要考察因素,归一化法合并产品收率及反应时间为评价指标,采用Statistica 6.0及SAS软件进行试验设计并分析试验结果。反应温度及介质固液比对试验结果影响显著,并确定酸水解法制备野黄芩素的最优反应条件为固液比(g/L)15(0.15g灯盏乙素加入10m L95%乙醇)、反应温度80℃,在此条件下可通过较短时间得到较为理想的产物收率。CCD优化野黄芩素制备工艺直观、高效,值得推广应用。
To optimize the reaction conditions of processing scutellarein from scutellarin hydrolysis by CCD(central composite design), temperature and the solid-liquid ratio were selected as the main factors, and the product yield and reaction time were both opted as evaluation index, which presented as overall desirability by relevant calculation. Statistica 6.0 and SAS software were used for statistic analysis of test results. The effect of reaction temperature and solid-liquid ratio on test results was significant.The optimal preparation conditions of scutellarin by acid hydrolysis were solid liquid ratio(g/L) 15, reaction temperature 80 ℃, and an ideal yield could be obtained in a short time under these conditions.The optimization ofprocessing conditions of scutellarein by CCD is intuitive and efficient, which is worthy of popularization and application.
To optimize the reaction conditions of processing scutellarein from scutellarin hydrolysis by CCD(central composite design), temperature and the solid-liquid ratio were selected as the main factors, and the product yield and reaction time were both opted as evaluation index, which presented as overall desirability by relevant calculation. Statistica 6.0 and SAS software were used for statistic analysis of test results. The effect of reaction temperature and solid-liquid ratio on test results was significant.The optimal preparation conditions of scutellarin by acid hydrolysis were solid liquid ratio(g/L) 15, reaction temperature 80 ℃, and an ideal yield could be obtained in a short time under these conditions.The optimization ofprocessing conditions of scutellarein by CCD is intuitive and efficient, which is worthy of popularization and application.
引文
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[2]王彪,袁娜,张永虎,等.野黄芩素通过PI3K/Nrf2/HO-1途径减轻LPS诱导的大鼠急性肺损伤[J].中南医学科学杂志,2016,44(4):409-413.
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[4]Shi X J,Chen GF,Liu X Q, et al.Scutellarein inhibits cancer cell metastasis in vitro and attenuates the development of fibrosarcoma in vivo[J].International journal of molecular medicine,2015, 35(1):31-38.
[5]静广平,吕克文,张晗,等.野黄芩素协同ABT-737抗头颈鳞癌作用的研究[J].口腔医学研究,2016,32(11):1188-1192.
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[13]周荣光,晏泽宇,赵加强,等.野黄芩素的制备、纯化与结构表征[J].光谱实验室,2011,28(5):2403-2406.
[14]Liu X R, Dong Y, Sun Y H, et al.Study on extraction technique of total isoflavones from kudzu rootand mensuration and TLC methods[J]. Food research and developent, 2006, 27(10):126-129.
[15]李富强,毛坤军,周萍,等.半枝莲的质量标准研究[J].中国药房,2015,26(21):2980-2982.
[16]Mezghani O, Ke X, Bourkaib N, et al.Optimized self-microemulsifying drug delivery systems(SMEDDS)for enhanced oral bioavailability of astilbin[J].Die Pharmazie,2011,66(10):754-760.
[17]Heoh J,Row K H.Central composite design for optimized extraction of polysaccharides from Undaria pinnatifida[J].Chemical research in Chinese university, 2012, 28(4):620-623.
[18]Hao J F, Wang F G, Wang X D, et al.Development and optimization of baicalin-loaded solid lipid nanoparticles prepared by coacervation method using central composite design[J].European journal of pharmaceutical sciences,2012, 47(2):497-505.
[19]Wu W, Cui G H, Lu B.Optimization of multiple evariables:application of central composite design and overall desirability[J].Chinese pharmaceutical journal,2000,35(8):530-533.
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[21]Sun C P, Gao W P, Zhao B Z, et al.Optimization for preparation of lemon-catalyzed ginsenoside Rg3 by response surface method[J].Chinese herbal medicines,2013,5(3):217-223.
[22]陈欣,陈光英,陈文豪,等.蓝花黄芩的黄酮成分及生物活性研究[J].中药材,2016,39(10):2240-2243.
[23]徐怀德,陈佳,包蓉,等.大孔吸附树脂分离纯化洋葱皮黄酮的研究[J].食品科学,2011,32(12):133-138.
[24]余沙,何珺,钱一鑫,等.银杏叶提取物中银杏黄酮苷元的提纯工艺研究[J].华西药学杂志,2011,26(6):577-579.
[25]Li N, Huang J M, Weng W Y, et al.Preparation and identification of scutellarein by HPLC with an enzymolysis reaction[J].Journal of liquid chromatography and related technologies,2006,29(9):1297-1306.
[26]聂朝霞.反相高效液相色谱法测定灯盏细辛中灯盏乙素含量[J].中国药业,2013,22(23):15-16.
[27]Huang J M, Li N, Yu Y Q, et al.Determination of aglycone conjugated metabolites of scutellarin in rat plasma by HPLC[J].Journal of pharmaceutical and biomedical analysis,2016,40(2):465-471.
[2]王彪,袁娜,张永虎,等.野黄芩素通过PI3K/Nrf2/HO-1途径减轻LPS诱导的大鼠急性肺损伤[J].中南医学科学杂志,2016,44(4):409-413.
[3]Sung N Y, Kim M Y, Li N G, et al.Scutellarein reduces inflammatory responses by inhibiting Src kinase activity[J].Korean J Physiol Pharmacol,2015,19(5):441-449.
[4]Shi X J,Chen GF,Liu X Q, et al.Scutellarein inhibits cancer cell metastasis in vitro and attenuates the development of fibrosarcoma in vivo[J].International journal of molecular medicine,2015, 35(1):31-38.
[5]静广平,吕克文,张晗,等.野黄芩素协同ABT-737抗头颈鳞癌作用的研究[J].口腔医学研究,2016,32(11):1188-1192.
[6]Tang H,Li N G,Tang Y P, et al.Identification of scutellarein metabolites in rat using ultra performance liquid chromatography/quadruple-time-of-flight mass spectrometry[J].The royal society of chemistry,2014,6(13):4667-4673.
[7]张铁英.灯盏花素化学组成及在大鼠体内代谢研究[D].沈阳:沈阳药科大学,2004.
[8]Dong Z X, Li N G, Zhang P X, et al.An Efficient chemical synthesis of scutellarein:an in vivo metabolite of scutellarin.[J].Molecules,2016,21(3):263.
[9]王晶,刘湘,董保平,等.野黄芩素的合成与表征[J].化学研究与应用,2012,3(6):480-483.
[10]凌成利,杨兆祥,张伟.灯盏花乙素苷元的制备研究进展[J].化学试剂,2015,37(2):132-134.
[11]郑晨,沈琪华,董志红,等.微生物转化灯盏乙素制备野黄芩素的研究[J].中国医药生物技术,2016,11(6):521-525.
[12]廖霞俐,易东,张淼,等.灯盏花乙素水解制备野黄芩素[J].昆明理工大学学报,2013,38(6):102-106.
[13]周荣光,晏泽宇,赵加强,等.野黄芩素的制备、纯化与结构表征[J].光谱实验室,2011,28(5):2403-2406.
[14]Liu X R, Dong Y, Sun Y H, et al.Study on extraction technique of total isoflavones from kudzu rootand mensuration and TLC methods[J]. Food research and developent, 2006, 27(10):126-129.
[15]李富强,毛坤军,周萍,等.半枝莲的质量标准研究[J].中国药房,2015,26(21):2980-2982.
[16]Mezghani O, Ke X, Bourkaib N, et al.Optimized self-microemulsifying drug delivery systems(SMEDDS)for enhanced oral bioavailability of astilbin[J].Die Pharmazie,2011,66(10):754-760.
[17]Heoh J,Row K H.Central composite design for optimized extraction of polysaccharides from Undaria pinnatifida[J].Chemical research in Chinese university, 2012, 28(4):620-623.
[18]Hao J F, Wang F G, Wang X D, et al.Development and optimization of baicalin-loaded solid lipid nanoparticles prepared by coacervation method using central composite design[J].European journal of pharmaceutical sciences,2012, 47(2):497-505.
[19]Wu W, Cui G H, Lu B.Optimization of multiple evariables:application of central composite design and overall desirability[J].Chinese pharmaceutical journal,2000,35(8):530-533.
[20]Zhang W L,Wang Y J,Gao X M,et al.Optimization of Jiawei Qing'e oral fast disintegrating tablets based on response surface-central composite design[J]. Chinese herbal medicines,2013,5(2):138-144.
[21]Sun C P, Gao W P, Zhao B Z, et al.Optimization for preparation of lemon-catalyzed ginsenoside Rg3 by response surface method[J].Chinese herbal medicines,2013,5(3):217-223.
[22]陈欣,陈光英,陈文豪,等.蓝花黄芩的黄酮成分及生物活性研究[J].中药材,2016,39(10):2240-2243.
[23]徐怀德,陈佳,包蓉,等.大孔吸附树脂分离纯化洋葱皮黄酮的研究[J].食品科学,2011,32(12):133-138.
[24]余沙,何珺,钱一鑫,等.银杏叶提取物中银杏黄酮苷元的提纯工艺研究[J].华西药学杂志,2011,26(6):577-579.
[25]Li N, Huang J M, Weng W Y, et al.Preparation and identification of scutellarein by HPLC with an enzymolysis reaction[J].Journal of liquid chromatography and related technologies,2006,29(9):1297-1306.
[26]聂朝霞.反相高效液相色谱法测定灯盏细辛中灯盏乙素含量[J].中国药业,2013,22(23):15-16.
[27]Huang J M, Li N, Yu Y Q, et al.Determination of aglycone conjugated metabolites of scutellarin in rat plasma by HPLC[J].Journal of pharmaceutical and biomedical analysis,2016,40(2):465-471.