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Separation method of salidroside and impurity therein and RP-HPLC analytical method of salidroside and impurity therein

A technology for salidroside and impurities, which is applied in the field of separation of salidroside and its impurities and the RP-HPLC analysis method of salidroside and its impurities, can solve the problems of poor separation effect and the like, and achieve a simple and reliable method Effect

Inactive Publication Date: 2009-02-04
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Generally, silica gel column chromatography is used for the separation of drug impurities, but the separation effect of this method is poor.

Method used

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  • Separation method of salidroside and impurity therein and RP-HPLC analytical method of salidroside and impurity therein
  • Separation method of salidroside and impurity therein and RP-HPLC analytical method of salidroside and impurity therein
  • Separation method of salidroside and impurity therein and RP-HPLC analytical method of salidroside and impurity therein

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1. Silica gel column chromatography enriches impurity

[0052] Sample mixing: Weigh an appropriate amount of 100-mesh silica gel and pour it into an evaporating dish, then pour an appropriate amount of salidroside with a saturated methanol solution of about 97% to cover it just right (the ratio of sample to silica gel is 1:0.68, w / w ), stirred evenly to evaporate most of the methanol, and dried to constant weight in a vacuum oven at 60°C.

[0053] Column packing: Wet packed 225g of 200-300 mesh silica gel with chloroform and equilibrated.

[0054] Sample loading: Take 8.5g sample-mixed silica gel (approximately equivalent to 5g sample) and add it to the top of the chromatographic column.

[0055] Elution: Chloroform:methanol gradient elution (14:1→10:1→6:1), flow rate is 3-4 drops / second, collected in 4 sections.

Embodiment 2

[0056] Embodiment 2. High performance liquid chromatography prepares impurity

[0057] 2.1 Selection of semi-preparative HPLC conditions

[0058] Preparation of the test solution: take an appropriate amount of salidroside raw material with a content of about 97%, add methanol to make a solution containing 0.2g per 1mL, use it as the test solution, filter it with a microporous membrane, and inject samples under different conditions .

[0059] 2.1.1 Detection wavelength

[0060] Using UV-2450 UV-Vis spectrophotometer to scan continuously at 200-400nm, it can be seen that salidroside has the maximum absorption at 275nm, and HEPG, HPAG and PAPG have strong absorption at 270, 280 and 265 respectively. Taking into account the sensitivity of the determination of the three, so the detection wavelength is selected as 275nm (see Figure 1).

[0061] 2.1.2 Columns

[0062] Due to the different fillers used in the chromatographic columns of different manufacturers, the column efficienc...

Embodiment 3

[0075] Example 3. Structure Identification

[0076] 3 impurity all through infrared spectrum (IR), mass spectrometry (MS), nuclear magnetic resonance spectrum ( 1 H NMR, 13 C NMR, 1 H- 1 Characterized by H COZY, DEPT, HSQC and HMBC), its spectral data are consistent with those of icariin, p-hydroxyphenylacetoxy-β-D-glucopyranoside and sprucetin reported in the literature [see: Toshio Miyase; Akira Ueno; Nobuo Takizawa. Phytochemistry. 1989, 28, 3484-3485. Pan, H.-F. Phytochemistry. 1995, 39, 1423-1428. Roger, A.D.; Lucia, V.H.; , 25, 1201-1204], which were determined to be icariside, p-hydroxyphenylacetoxy-β-D-glucopyranoside, and sprucetin, respectively.

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Abstract

The invention discloses a separation method of salidroside impurities which includes the steps of first separation with silica gel column chromatography, elution with chloroform-ethanol gradients, collection by four sections and the separation and purification with semi-preparative high-performance liquid chromatography; wherein, the semi-preparative high-performance liquid chromatography is provided with the conditions as follows: a chromatographic column: ODS C18, 5mum and 250 * 10.0mm (I. D.); volume ratios of components of mobile phases: methanol to water equals to 11 to 89; flow rate: 3.0 mL / min; column temperature: 25 DEG C; detection wavelength: UV275nm; sample size: 50 muL; effluent liquid collection by section. The high-performance liquid chromatography of the salidroside and impurities thereof adopt the reversed-phase high-performance liquid chromatography with the following chromatographic conditions: a chromatographic column: ODS C18, 5mum and 150 * 4.6mm (I. D.); mobile phases: methanol to water equals to 15 to 85; flow rate: 1.0 mL / min; column temperature: 25 DEG C; detection wavelength: UV275nm; sample size: 20 muL. The contents of the salidroside and the impurities HEPG, HPAG and PAPG of the salidroside samples can be determined accurately and simultaneously by adopting the high performance liquid chromatography of the salidroside and impurities thereof, which provides a simple and reliable method for the quality control analysis in the production process.

Description

technical field [0001] The invention relates to the separation of salidroside and its three impurities and its high-performance liquid chromatography analysis method. Background technique [0002] Salidroside, English name salidroside, chemical name "p-hydroxyphenethyl-β-D-glucopyranoside (p-hydroxyphenethyl-β-D-glucoside)", systematic name: 1-(4-hydroxy)benzene Ethyl-β-D-glucopyranoside is mainly extracted from the plateau medicinal plant "Rhodiola sachalinensis" and the commonly used traditional Chinese medicine "Ligustrum lucidum" [Xu ​​Baojun, Zheng Yinan, Li Xianggao. New progress in the research of Rhodiola plants. Chinese Medicinal Materials, 2000, 23(9): 580-584; Shi Lifu, Cai Qin, Cao Yingying, et al. Chemical constituents and pharmacological effects of the traditional Chinese medicine Ligustrum lucidum. Journal of Pharmaceutical Practice, 1997 , 15(4):197-200]. Pharmacological experiments show that salidroside, an extract of Rhodiola rosea, has good effects on th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/18G01N30/02
Inventor 都述虎彭艳罗晶陆庆陈立娜李飞杨伟
Owner NANJING MEDICAL UNIV
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