近红外光谱法快速测定怀地黄中总苯乙醇苷、总环烯醚萜苷的含量
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摘要
目的:建立快速测定怀地黄中总苯乙醇苷及总环烯醚萜苷含量的方法。方法:采用紫外-可见分光光度法测定药材样品中总苯乙醇苷及总环烯醚萜苷的含量。采用近红外光谱法结合偏最小二乘法,最佳光谱预处理方法分别为多元散射校正法联合一阶导数法、标准归一化法联合一阶导数法,最佳光谱范围分别为6 703.35～11 065.54 cm~(-1)、3 999.63～9 102.36 cm~(-1),最佳主因子数分别为10、7,建立药材样品中总苯乙醇苷及总环烯醚萜苷含量的定量分析模型。结果:药材样品中总苯乙醇苷及总环烯醚萜苷含量测定方法学经验证符合要求。总苯乙醇苷、总环烯醚萜苷定量模型的校正集内部交叉验证相关系数分别为0.998 2、0.980 9,校正均方根偏差分别为0.032 7、0.186 0,预测均方根偏差分别为0.035 5、0.035 1,交叉验证均方根偏差分别为0.256 9、0.574 3。总苯乙醇苷、总环烯醚萜苷含量的预测值分别为0.268%～1.636%、3.424%～6.978%,测定值分别为0.299%～1.629%、3.431%～6.952%,绝对偏差分别为-0.042%～0.067%、-0.111%～0.088%,相对偏差分别为-0.819%～0.076%、-2.257%～1.672%,预测值与测定值比较差异均无统计学意义(P>0.05)。结论:该方法快速准确、简便,可用于不同种质怀地黄中总苯乙醇苷及总环烯醚萜苷含量的测定。
OBJECTIVE:To establish a method for rapid determination of total phenylethanoid glycosides and total iridoid glycosides in the root of Rehmannia glutinosa. METHODS:The contents of total phenylethanoid glycosides and total iridoid glycosides in medicinal material samples were determined by UV spectrophotometry. Quantitative model of total phenylethanoid glycosides and total iridoid glycosides in medicinal samples was established by NIRS-PLS method. The optimal pretreatment spectra were multivariate scattering correction combined with first derivative method,standard normalization combined with first derivative method. The optimum spectral ranged from 6 703.35-11 065.54 cm~(-1)and 3 999.63-9 102.36 cm~(-1). The optimum principal factor number were 10 and 7. RESULTS:The content determination of total phenylethanoid glycosides and total iridoid glycosides in medicinal material samples was proved to meet the requirements by methodological experience. The internal cross validation determination coefficients of total phenylethanoid glycosides and total iridoid glycosides were 0.998 2 and 0.980 9. The correction of root mean square error was 0.032 7 and 0.186 0. The root mean square error of prediction were 0.035 5 and 0.035 1. The root mean square error of cross validation were 0.256 9 and 0.574 3. The predicted values of total phenylethanol glycosides and total iridoid glycosides were 0.268%-1.636% and 3.424%-6.978%,respectively;the determination value of them were 0.299%-1.629%and 3.431%-6.952%,respectively;the absolute deviations were-0.042%-0.067% and-0.111%-0.088%,respectively;the relative deviations were-0.819%-0.076% 、-2.257%-1.672%,respectively;There was no statistical significance between predicted values and measured values(P>0.05). CONCLUSIONS:The method is accurate and simple. The method can be used for the rapid determination of total phenylethanoid glycosides and total iridoid glycosides in different germplasms of R. glutinosa.
OBJECTIVE:To establish a method for rapid determination of total phenylethanoid glycosides and total iridoid glycosides in the root of Rehmannia glutinosa. METHODS:The contents of total phenylethanoid glycosides and total iridoid glycosides in medicinal material samples were determined by UV spectrophotometry. Quantitative model of total phenylethanoid glycosides and total iridoid glycosides in medicinal samples was established by NIRS-PLS method. The optimal pretreatment spectra were multivariate scattering correction combined with first derivative method,standard normalization combined with first derivative method. The optimum spectral ranged from 6 703.35-11 065.54 cm~(-1)and 3 999.63-9 102.36 cm~(-1). The optimum principal factor number were 10 and 7. RESULTS:The content determination of total phenylethanoid glycosides and total iridoid glycosides in medicinal material samples was proved to meet the requirements by methodological experience. The internal cross validation determination coefficients of total phenylethanoid glycosides and total iridoid glycosides were 0.998 2 and 0.980 9. The correction of root mean square error was 0.032 7 and 0.186 0. The root mean square error of prediction were 0.035 5 and 0.035 1. The root mean square error of cross validation were 0.256 9 and 0.574 3. The predicted values of total phenylethanol glycosides and total iridoid glycosides were 0.268%-1.636% and 3.424%-6.978%,respectively;the determination value of them were 0.299%-1.629%and 3.431%-6.952%,respectively;the absolute deviations were-0.042%-0.067% and-0.111%-0.088%,respectively;the relative deviations were-0.819%-0.076% 、-2.257%-1.672%,respectively;There was no statistical significance between predicted values and measured values(P>0.05). CONCLUSIONS:The method is accurate and simple. The method can be used for the rapid determination of total phenylethanoid glycosides and total iridoid glycosides in different germplasms of R. glutinosa.
引文
[1]谢彩侠,李雅静,张苗,等.怀地黄中地黄苷A、地黄苷D及益母草苷含量快速分析方法的建立[J].中国实验方剂学杂志,2018,24(6):47-54.
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[4]谢彩侠,李雅静,张苗,等.不同种质地黄块根菊花心与非菊花心部位有效成分特征分析[J].中国实验方剂学杂志,2018,24(20):75-83.
[5]易满,封传华,汤小林,等.不同产地车前草中总苯乙醇苷和毛蕊花糖苷含量测定[J].中国中医药信息杂志,2017,24(9):84-86.
[6]吉雪琪,孙鹏,祁建军,等.地黄生长期根叶中梓醇及总环烯醚萜苷含量变化[J].中国中药杂志,2014,39(3):466-469.
[7]陈瑾,谭丽媛,李敏,等.冻干鲜地黄生地黄中梓醇和毛蕊花糖苷的含量比较[J].时珍国医国药,2018,29(7):1625-1627.
[8] SASAKI H,NISHIMURA H,CHIN M,et al. Nine phenethyl alcohol glycosides from Stachys sieboldii[J]. Phytochemistry,1989,28(30):875-877.
[9]刘彦飞,赵宇,温学森,等.梓醇的药效学及化学转化研究现状[J].中国中药杂志,2007,32(12):1128-1130
[10]杨云,张华锋,刘炯,等.道地产区不同品种怀地黄中梓醇及毛蕊花糖苷的含量比较[J].中国实验方剂学杂志,2013,19(16):97-101.
[11]王丰青,王丽娜,智惊宇,等.不同品种地黄中毛蕊花糖苷的动态积累规律变化[J].中国实验方剂学杂志,2017,23(24):78-83.
[12]谢彩侠,左春芳,白雁,等.近红外光谱技术快速测定盾叶薯蓣中伪原薯蓣皂苷的含量[J].中国药房,2013,24(15):1396-1399.
[13]张迪文,白雁,谢彩侠,等.近红外光谱法快速测定女贞子药材中女贞苷的含量[J].中国药房,2016,27(36):5140-5143.
[14]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京:中国医药科技出版社,2015:374-377.
[15]封传华,任琦,汤小林,等.车前草中总苯乙醇苷及毛蕊花糖苷的含量测定[J].中国药师,2017,20(8):1477-1479.
[2] ZHANG RX,LI MX,JIA ZP. Rehmannia glutlnosa:review of botany,chemistry and pharmacology[J]. J Ethnopharmacol,2008,117(2):199-214.
[3]张汝学,贾正平,李茂星,等.地黄寡糖对2型糖尿病大鼠外周血像、激素水平和胰岛病理学的影响[J].西北国防医学杂志,2009,30(3):161-164.
[4]谢彩侠,李雅静,张苗,等.不同种质地黄块根菊花心与非菊花心部位有效成分特征分析[J].中国实验方剂学杂志,2018,24(20):75-83.
[5]易满,封传华,汤小林,等.不同产地车前草中总苯乙醇苷和毛蕊花糖苷含量测定[J].中国中医药信息杂志,2017,24(9):84-86.
[6]吉雪琪,孙鹏,祁建军,等.地黄生长期根叶中梓醇及总环烯醚萜苷含量变化[J].中国中药杂志,2014,39(3):466-469.
[7]陈瑾,谭丽媛,李敏,等.冻干鲜地黄生地黄中梓醇和毛蕊花糖苷的含量比较[J].时珍国医国药,2018,29(7):1625-1627.
[8] SASAKI H,NISHIMURA H,CHIN M,et al. Nine phenethyl alcohol glycosides from Stachys sieboldii[J]. Phytochemistry,1989,28(30):875-877.
[9]刘彦飞,赵宇,温学森,等.梓醇的药效学及化学转化研究现状[J].中国中药杂志,2007,32(12):1128-1130
[10]杨云,张华锋,刘炯,等.道地产区不同品种怀地黄中梓醇及毛蕊花糖苷的含量比较[J].中国实验方剂学杂志,2013,19(16):97-101.
[11]王丰青,王丽娜,智惊宇,等.不同品种地黄中毛蕊花糖苷的动态积累规律变化[J].中国实验方剂学杂志,2017,23(24):78-83.
[12]谢彩侠,左春芳,白雁,等.近红外光谱技术快速测定盾叶薯蓣中伪原薯蓣皂苷的含量[J].中国药房,2013,24(15):1396-1399.
[13]张迪文,白雁,谢彩侠,等.近红外光谱法快速测定女贞子药材中女贞苷的含量[J].中国药房,2016,27(36):5140-5143.
[14]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京:中国医药科技出版社,2015:374-377.
[15]封传华,任琦,汤小林,等.车前草中总苯乙醇苷及毛蕊花糖苷的含量测定[J].中国药师,2017,20(8):1477-1479.