成分分析

HPLC-ELSD法同时测定地黄及其不同炮制品中8个糖类成分的含量*

展开
  • 河南中医药大学 河南省中药资源与中药化学重点实验室,郑州 450046
第一作者 Tel:(0371)65676686;E-mail:sjxue3901@163.com
**Tel:(0371)65676686;E-mail:suiqingchen@sohu.com

修回日期: 2023-05-08

  网络出版日期: 2024-06-25

基金资助

*国家自然科学基金面上项目(81973477);河南省中医药科学研究专项课题重大专项(2022ZYZD18)

Simultaneous determination of eight saccharides contents in Radix Rehmanniae and its different processed products by HPLC-ELSD*

Expand
  • Henan University of Chinese Medicine, Henan Provincial Key Laboratory of Chinese Medicine Resources and Chinese Medicine Chemistry, Zhengzhou 450046, China

Revised date: 2023-05-08

  Online published: 2024-06-25

摘要

目的: 建立高效液相色谱-蒸发光散射检测器法同时测定地黄及其不同炮制品中8个糖类成分的含量,分析地黄炮制前后糖类成分的含量变化情况。方法: 采用XBridgeBEH Amide色谱柱(250 mm×4.6 mm,5 μm);30%乙腈水+0.1%氨水(A)和90%乙腈水+0.1%氨水(B)为流动相,梯度洗脱;柱温40 ℃;漂移管温度105 ℃;气体流量2.0 L·min-1;增益值为1;进样量为10 μL。结果: 8个糖类成分在各自浓度范围内线性关系良好(r>0.999 0),精密度、稳定性、重复性试验结果的RSD均<3.0%,平均加样回收率为 97.7%~101.3%。采用主成分分析和方差分析对上述8个糖类成分的含量进行分析,结果显示地黄及其不同炮制品样品中主要含有糖的种类和含量均存在显著差异。结论: 该方法简单、准确、重现性好,能有效分析地黄及其不同炮制品中8个糖类成分的含量,为地黄药材的质量控制提供了参考依据。

本文引用格式

薛淑娟, 陈越, 陈随清, 车奇涛 . HPLC-ELSD法同时测定地黄及其不同炮制品中8个糖类成分的含量*[J]. 药物分析杂志, 2023 , 43(6) : 939 -949 . DOI: 10.16155/j.0254-1793.2023.06.04

Abstract

Objective: To establish an high performance liquid chromatography evaporative light scattering detection (HPLC-ELSD) method for simultaneous determination of eight saccharides contents in Radix Rehmanniae (RR) and its different processed products and to analyze the changes of saccharides contents before and after RR processing. Methods: Determination was carried out on a Waters XBridgeBEH Amide column (250 mm×4.6 mm, 5 μm). The mobile phase was composed of 90% acetonitrile containing 0.1% ammonia (B) and 30% acetonitrile containing 0.1% ammonia (A) with gradient elution. The column temperature was 40 ℃ and the injection volume was 10 μL. Furthermore, the drift tube temperature, carrier gas flow rate and gain value of evaporative light scattering detection were set at 105 ℃, 2.0 L·min-1 and 1, respectively. Principal component analysis (PCA) and variance analysis (ANOVA) were used to analyze the contents of the above eight saccharides components. Results: Good separation of 8 components was achieved within 64 min and calibration curves of the eight components showed good linear relationship (r>0.999 0). The RSDsof precision,stability and repeatability results were all less than 3.00%, and the average recoveries were within 97.7%-101.3%. PCA and ANOVA results showed that the types and contents of the main saccharides in RR and its different processed products were significantly different. Conclusion: The method is simple, accurate and reproducible, and can effectively analyze the contents of eight saccharides in RR and its different processed products, which provides a reference for the quality control of RR.

参考文献

[1] 中华人民共和国药典2020年版. 一部[S].2020:129
ChP 2020. Vol Ⅰ[S].2020:129
[2] 陈金鹏, 张克霞, 刘毅, 等. 地黄化学成分及药理作用研究进展[J].中草药, 2021, 52(6):1772
CHEN JP, ZHANG KX, LIU Y, et al. Research progress on chemical constituents and pharmacological actions of Radix Rehmannia[J].Chin Tradit Herb Drugs, 2021, 52(6):1772
[3] 王悦, 周巧, 张学兰, 等. HPLC法同时测定地黄及不同炮制品中8个成分的含量[J].中药材, 2021, 44(1):64
WANG Y, ZHOU Q, ZHANG XL, et al. Simultaneous determination of eight compounds contents of rehmanniae radix and its different processed products by HPLC[J].J Chin Med Mater, 2021, 44(1):64
[4] 朱珏, 朱香梅, 石雨荷, 等. 地黄的研究进展及其质量标志物的预测分析[J].中药材. 2022,45(5):1291
ZHU Y, ZHU XM, SHI YH, et al. Research progress on Radix Rehmannia and predictive analysis on its Q-Marker[J].J Chin Med Mater, 2022,45(5):1291
[5] 宋琳琳, 薛淑娟, 王利丽, 等. 不同储藏年限地黄化学成分分析[J].中成药, 2020, 42(10):2661
SONG LL, XUE SJ, WANG LL, et al. Analysis of chemical constituents from Radix Rehmannia with different storage years[J].Chin Tradit Pat Med, 2020, 42(10):2661
[6] 张留记,王建霞,屠万倩,等. 生地黄与熟地黄中5个苷类成分和总多糖的含量比较[J].天然产物研究与开发, 2019, 31(4):5661
ZHANG LJ, WANG JX, TU WQ, et al. Comparation of the contents of 5 glycosides and total polysaccharides in Rehmanniae Radix and Rehmanniae Radix Praeparata[J].Nat Prod Res Dev, 2019, 31(4):566
[7] 严斐霞, 谢永艳, 陈畅, 等. 熟地黄炮制过程中的化学成分变化和药理作用研究进展[J].时珍国医国药. 2021,32(10):2493
YAN FX, XIE YY, CHEN C, et al. Research Progress of the changes in chemical composition and pharmacological actions in the proceeding of Rehmanniae Radix Praeparata[J].Lishizhen Med Mater Med Res, 2021,32(10):2493
[8] 张文婷, 何佳, 郭增喜, 等. HPLC-ELSD特征图谱分析地黄炮制过程成分变化[J].中国中药杂志, 2020, 45(16):3877
ZHANG WT, HE J, GUO ZX, et al. Ingredients changes in Rehmanniae Radix processing based by HPLC-ELSD specific chromatogram[J].China J Chin Mater Med, 2020, 45(16):3877
[9] 王晓尧, 崔璨, 刘雅琳, 等. 鲜地黄及其多糖对实热大鼠焦虑模型影响的研究[J].中药药理与临床, 2021, 37(6):95
WANG XY, CUI C, LIU YL, et al. Effect of fresh Dihuang and its polysaccharide on anxiety model in rats with shire syndrome[J].Pharmacol Clin Chin Mater Med, 2021, 37(6):95
[10] 周艳, 杜莉杰, 郑旭亚, 等. 基于古法特色炮制前后的地黄饮片及其多糖对衰老模型大鼠的抗氧化作用比较[J].中国药房, 2020, 31(17):2087
ZHOU Y, DU LJ, ZHENG XY, et al. Comparison of antioxidant effect of radix rehmannia decoction pieces and its polysaccharides on aging model rats before and after processing based on the characteristic ancient method[J].China Pharm, 2020, 31(17):2087
[11] 李玉丹, 黄河勋, 周洋洋, 等. GC-MS法同时检测南瓜果实肌醇类和单、双糖类物质的研究[J].食品科技, 2017, 42(5):279
LI YD, HUANG HX, ZHOU YY, et al. Simultaneously quantifying inositols and mono-, di-saccharides in pumpkin fruit by GC-MS method[J].Food Sci Technol, 2017, 42(5):279
[12] 景海漪, 史辑, 崔妮, 等. 巴戟天炮制前后寡糖类成分HPLC-CAD指纹图谱研究[J].中草药, 2014, 45(10):1412
JING HY, SHI J, CUI N, et al. Fingerprints of oligosaccharides in Morinda officinalis before and after processing by HPLC-CAD[J].Chin Tradit Herb Drugs, 2014, 45(10):1412
[13] 刘美廷,赵静,李绍平. 毛细管电泳在中药糖类成分分析中的研究进展[J].药物分析杂志, 2020, 40(10):1727
LIU MY, ZHAO J, LI SP. Research advance of capillary electrophoresis on the analysis of saccharides from traditional Chinese medicine[J].Chin J Pharm Anal, 2020, 40(10):1727
[14] MANTOVANI V, GALEOTTI F, MACCARI F, et al. Recent advances in capillary electrophoresis separation of monosaccharides, oligosaccharides, and polysaccharides[J].Electrophoresis, 2018, 39(1):179
[15] XUE SJ, WANG LL, CHEN SQ, et al. Simultaneous analysis of saccharid es between fresh and processed radix rehmanniae by HPLC and UHPLC-LTQ-Orbitrap-MS with multivariate statistical analysis[J].Molecules, 2018, 23(3):541
[16] 薛淑娟, 陈随清. 基于代谢组学分析不同蒸制次数熟地黄中糖类成分的变化规律[J].中国实验方剂学杂志, 2018, 24(22):1
XUE SJ, CHEN SQ. Analysis on change rule of carbohydrates in rehmanniae radix praeparata with different processing times based on metabolomics[J].Chin J Exp Tradit Med Form, 2018, 24(22):1
[17] 雷金艳, 贾建伟. 地黄中水苏糖的研究进展[J].医学综述,2010,16(6):935
LEI JY, JIA JW. Research progress in the stachyose in rehmannia glutimosa[J].Med Recap, 2010, 16(6):935
文章导航

/