基于化学成分变化优化麦冬硫熏工艺
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摘要
目的基于麦冬经不同程度硫熏后,相关检测指标的变化情况,优化麦冬硫熏的适宜工艺。方法运用苯酚-硫酸法测定麦冬多糖的量;运用HPLC-ELSD法测定麦冬皂苷D和D′的量,流动相为乙腈-水(50∶50),漂移管温度40℃,氮气体积流量2.0 L/min;运用HPLC-UV法进行麦冬正丁醇部位指纹图谱研究,流动相为乙腈-0.1%磷酸水梯度洗脱,检测波长297 nm,同法测定甲基麦冬二氢高异黄酮A和B的量。以硫熏麦冬的总多糖、麦冬皂苷D和D′、甲基麦冬二氢高异黄酮A和B的质量分数及指纹图谱得分为综合考察指标,以硫磺用量和硫熏时间为考察因素,运用星点设计-效应面法优化麦冬硫熏工艺。结果在实验设计范围内,随着硫磺用量和硫熏时间的增加,多糖的量先增加后降低,麦冬皂苷D和D′的量轻微增加后降低,甲基麦冬二氢高异黄酮A和B的量逐步降低。最终确定麦冬硫熏工艺为硫磺用量120~200 g/m~3,硫熏时间0.6~1.5 h,多元2项式方程为Y=0.574+0.054 3 X_1-0.008 13 X_2-0.518 X_(12)+0.131 X_(22)+0.153 X_1X_2,R-Sq=0.971。工艺验证结果表明偏差绝对值小于3%。结论本研究明确麦冬硫熏后相关化学成分变化情况,建立适宜麦冬的硫熏工艺。
Objective To optimize the suitable technology of Ophiopogon japonicus(OJ) fumigation based on the changes of relative indexes after the different levels of sulfur fuming. Methods The phenol-sulfuric acid method was used to determine the content of polysaccharide. HPLC-ELSD method was used to determine the contents of Ophiopogon saponins D(OPD) and D'(OPD′) with the mobile phase of acetonitrile-water(50∶50), drift tube temperature at 40 ℃, and nitrogen volumetric flow of 2.0 L/min. The fingerprints of OJ were determined by HPLC-UV method, the mobile phase was eluted with acetonitrile-0.1% phosphoric acid gradient, and the detection wavelength was 297 nm. The contents of ethylophiopogonanones A(MA) and B(MB) were determined using the same method. Using the contents of total polysaccharides of OJ, OPD and OPD′, MA and MB, and the contents of other components in the fingerprints as control indexes, and the dosage of sulfur and the time of sulfur fumigation as factors, the central composite design-response surface methodology(CCD-RSM) was used to optimize sulfur fumigation process. Results In the experimental design range, the content of polysaccharides increased first and then decreased with the increase of sulfur dosage and sulfur fumigation time, and the contents of OPD and OPD′ increased slightly and then decreased. The contents of MA and MB were slightly reduced. The sulfur fuming process was determined as follows: sulfur dosage was 120—200 g/m3, sulfur fuming time was 0.6—1.5 h, binomial equation: Y = 0.574 + 0.054 3 X1-0.008 13 X2-0.518 X12 + 0.131X22 + 0.153 X1X2(R-Sq = 0.971). Process validation: the absolute value of deviation was less than 3%. Conclusion In this study, the changes of chemical composition of OJ were studied, and the sulfur smelting process suitable for OJ was established.
Objective To optimize the suitable technology of Ophiopogon japonicus(OJ) fumigation based on the changes of relative indexes after the different levels of sulfur fuming. Methods The phenol-sulfuric acid method was used to determine the content of polysaccharide. HPLC-ELSD method was used to determine the contents of Ophiopogon saponins D(OPD) and D'(OPD′) with the mobile phase of acetonitrile-water(50∶50), drift tube temperature at 40 ℃, and nitrogen volumetric flow of 2.0 L/min. The fingerprints of OJ were determined by HPLC-UV method, the mobile phase was eluted with acetonitrile-0.1% phosphoric acid gradient, and the detection wavelength was 297 nm. The contents of ethylophiopogonanones A(MA) and B(MB) were determined using the same method. Using the contents of total polysaccharides of OJ, OPD and OPD′, MA and MB, and the contents of other components in the fingerprints as control indexes, and the dosage of sulfur and the time of sulfur fumigation as factors, the central composite design-response surface methodology(CCD-RSM) was used to optimize sulfur fumigation process. Results In the experimental design range, the content of polysaccharides increased first and then decreased with the increase of sulfur dosage and sulfur fumigation time, and the contents of OPD and OPD′ increased slightly and then decreased. The contents of MA and MB were slightly reduced. The sulfur fuming process was determined as follows: sulfur dosage was 120—200 g/m3, sulfur fuming time was 0.6—1.5 h, binomial equation: Y = 0.574 + 0.054 3 X1-0.008 13 X2-0.518 X12 + 0.131X22 + 0.153 X1X2(R-Sq = 0.971). Process validation: the absolute value of deviation was less than 3%. Conclusion In this study, the changes of chemical composition of OJ were studied, and the sulfur smelting process suitable for OJ was established.
引文
[1]中国药典[S].一部.2015.
[2]苏雪梅,冷光.川麦冬的化学成分研究[J].中国药物与临床,2014,14(10):1364-1365.
[3]黄光辉,孙连娜.麦冬多糖的研究进展[J].现代药物与临床,2012,27(5):523-529.
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[5]童菊华,庞小存,王威,等.杭麦冬与川麦冬中高异黄酮类成分和抗氧化活性的比较[J].中草药,2015,46(20):3091-3095.
[6]何礼,金虹,梁雪兰,等.HPLC测定川麦冬块根及须根中的麦冬皂苷D[J].华西药学杂志,2014,29(5):583-584.
[7]缪菊连,黄照昌,王成军,等.HPLC-ELSD法测定生脉饮中麦冬皂苷D[J].中成药,2015,37(2):462-464.
[8]袁嘉瑞,汪春飞,宋捷,等.麦冬醇提物抑制肺癌生长及自噬作用研究[J].中草药,2016,47(9):1541-1547.
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[13]杜伟锋,张浩,岳显可,等.高效液相色谱法同时测定浙贝母硫熏前后8个水溶性成分的含量[J].中国药学杂志,2016,51(8):659-662.
[14]王赵,陈玉武,王琼,等.硫熏白芍的质量评价[J].中国中药杂志,2014,39(16):3074-3078.
[15]吴笑如,徐德生,冯怡,等.HPLC-ELSD测定川麦冬须根大孔树脂富集物中麦冬皂苷D、D′的含量[J].中成药,2006,28(11):1638-1640.
[16]王进,刘汉清,刘霖,等.HPLC定量指纹图谱法评价川麦冬质量研究[J].中药材,2013,36(5):721-725.
[17]李美云,雷小小,周江,等.星点设计-效应面法优化莲心总碱固体分散体渗透泵控释片处方[J].中草药,2016,47(18):3204-3210.
[18]张雪峰,杨轲,欧燕,等.星点设计-效应面法优化天山雪莲提取物磷脂复合物制备工艺[J].中草药,2014,45(16):2326-2332.
[19]岳国超,陈丽华,刘红宁,等.多指标综合评分法考察健胃消食片的流化制粒工艺[J].中草药,2014,45(7):949-954.
[2]苏雪梅,冷光.川麦冬的化学成分研究[J].中国药物与临床,2014,14(10):1364-1365.
[3]黄光辉,孙连娜.麦冬多糖的研究进展[J].现代药物与临床,2012,27(5):523-529.
[4]罗霄,张兴国,杨言琛,等.麦冬黄酮类成分的研究进展[J].中国中医药科技,2015,22(5):603-605.
[5]童菊华,庞小存,王威,等.杭麦冬与川麦冬中高异黄酮类成分和抗氧化活性的比较[J].中草药,2015,46(20):3091-3095.
[6]何礼,金虹,梁雪兰,等.HPLC测定川麦冬块根及须根中的麦冬皂苷D[J].华西药学杂志,2014,29(5):583-584.
[7]缪菊连,黄照昌,王成军,等.HPLC-ELSD法测定生脉饮中麦冬皂苷D[J].中成药,2015,37(2):462-464.
[8]袁嘉瑞,汪春飞,宋捷,等.麦冬醇提物抑制肺癌生长及自噬作用研究[J].中草药,2016,47(9):1541-1547.
[9]曹婷婷,孙志蓉,杨春宁,等.硫黄熏蒸中药材的研究现状分析[J].中国现代中药,2016,18(5):678-681.
[10]李铎.硫熏中药材快速检测装置设计研究[D].保定:河北大学,2016.
[11]汤坚,汪华君,蒋俊,等.基于主成分分析和硫熏前后无机元素含量变化的硫熏与非硫熏菊花鉴别方法[J].中国实验方剂学杂志,2014,20(13):97-101.
[12]刘丽芳.硫熏对山药的内在质量影响及无硫护色工艺研究[D].南昌:南昌大学,2016.
[13]杜伟锋,张浩,岳显可,等.高效液相色谱法同时测定浙贝母硫熏前后8个水溶性成分的含量[J].中国药学杂志,2016,51(8):659-662.
[14]王赵,陈玉武,王琼,等.硫熏白芍的质量评价[J].中国中药杂志,2014,39(16):3074-3078.
[15]吴笑如,徐德生,冯怡,等.HPLC-ELSD测定川麦冬须根大孔树脂富集物中麦冬皂苷D、D′的含量[J].中成药,2006,28(11):1638-1640.
[16]王进,刘汉清,刘霖,等.HPLC定量指纹图谱法评价川麦冬质量研究[J].中药材,2013,36(5):721-725.
[17]李美云,雷小小,周江,等.星点设计-效应面法优化莲心总碱固体分散体渗透泵控释片处方[J].中草药,2016,47(18):3204-3210.
[18]张雪峰,杨轲,欧燕,等.星点设计-效应面法优化天山雪莲提取物磷脂复合物制备工艺[J].中草药,2014,45(16):2326-2332.
[19]岳国超,陈丽华,刘红宁,等.多指标综合评分法考察健胃消食片的流化制粒工艺[J].中草药,2014,45(7):949-954.