Method for measuring weight-average molecular weight and content of polyguluronate sulfate

A technology of guluronic acid sulfate and weight-average molecular weight, which is applied in the field of natural medicinal chemistry and its quality control, can solve the problems of differences in structure and color rendering efficiency, the inability to accurately quantify acidic sugars, etc., and solve the problem of large measurement deviations Effect

Active Publication Date: 2019-03-12
GREEN VALLEY (SHANGHAI) PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no standard product for the monosaccharide of acidic sugar. If glucuronic acid is used as the standard product, its structure and color rendering efficiency are different from that of acidic sugar, and it is impossible to accurately quantify acidic sugar.

Method used

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  • Method for measuring weight-average molecular weight and content of polyguluronate sulfate
  • Method for measuring weight-average molecular weight and content of polyguluronate sulfate
  • Method for measuring weight-average molecular weight and content of polyguluronate sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] Example 1 SEC and ICP-MS reveal the separation mechanism of acidic sugars in size exclusion chromatography, and determine the weight average molecular weight and content of polyguluronic acid sulfate sodium salt

[0084] Step 1: SEC-ICP-MS to determine the peak position and content of metal ions

[0085] (1) Use the column Waters ACQUITY SEC 1.7um 4.6×150mm column, 0.08mol / L NH4Ac as mobile phase, flow rate 0.1mL / min.

[0086] (2) Combine SEC with ICP-MS: dissolve the sample in water, the concentration is 0.02mg / ml, inject 20ul, collect 23 Na, 43 Ca, 44 Ca signaling. Concentrations of 0.1ppm, 0.5ppm, 1.0ppm, 5.0ppm and 10.0ppm Na ion standard solutions were prepared respectively, and the content of metal ions in the sample (A value) was calculated by the external standard method. The results of A values ​​are shown in Table 1.

[0087] Step 2: Determination of weight average molecular weight and content by SEC-MALS

[0088] (1) Use the column Waters ACQUITY SE...

Embodiment 2

[0099] Embodiment 2 SEC-MALS measures the weight-average molecular weight and content of polyguluronic acid sulfate potassium salt

[0100] Step 1: Determination of the ratio of metal ions by ion chromatography

[0101] K ion standard solution is configured as 25, 10, 12.5, 6.25, 3.125ppm. The sample concentration was 2 mg / ml.

[0102] Ion chromatography conditions: pre-column: Metrosep C4Guard / 4.0; separation column: Metrosep

[0103] C5-150 / 4.0; mobile phase: ultrapure aqueous solution of 5mM nitric acid; flow rate: 0.9ml / min; injection volume 20ul. The content of metal ions was determined by external standard method.

[0104] Step 2: Determine dn / dc

[0105] (1) Weigh the sample with constant weight, and prepare a series of solutions with concentrations of 0.2mg / ml, 0.4mg / ml, 0.8mg / ml, 1.2mg / ml, 1.8mg / ml, and 2mg / ml with mobile phase.

[0106] (2) Manually inject mobile phase, 0.2mg / ml, 0.4mg / ml, 0.8mg / ml, 1.2mg / ml, 1.8mg respectively with a differential refractive ind...

Embodiment 3

[0115] Embodiment 3 SEC-MALS measures the weight-average molecular weight and content of polyguluronic acid sulfate calcium salt

[0116] Step 1: Determination of metal ion content by flame atomic absorption method:

[0117] Collect the spectral lines of Ca and prepare Ca standard solutions of 1mg / L, 10mg / L, 50mg / L, 75mg / L and 100mg / L; the concentration of the sample solution is prepared to be 200mg / L.

[0118] Step 2: Determine dn / dc

[0119] With embodiment 2 step 2. See Table 3 for the measured values.

[0120] Step 3: Determination of weight average molecular weight and content by SEC-MALS

[0121] (1) Use a chromatographic column Shodex OHpak SB-803HQ 7.8×300mm (Shodex), 0.15mol / L NaCl as the mobile phase, and a flow rate of 0.5mL / min.

[0122] (2) Combine SEC with MALS, in the mobile phase of the sample solution, the concentration is 10mg / ml, and the injection volume is 20ul, that is, the Y value in the formula is 200ug. The experimental results are shown in Table 3...

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Abstract

The invention belongs to the field of natural medicine chemistry and quality control, and relates to a method for measuring the weight-average molecular weight and the content of polyguluronate sulfate. Weight-average molecular weight and content results of the polyguluronate sulfate measured by an SEC-MALS (size exclusion chromatography with multi-angle laser scattering detector) are corrected byaid of the metal ion content of the polyguluronate sulfate. The weight-average molecular weight and the content of the polyguluronate sulfate can be rapidly and accurately measured by the method.

Description

technical field [0001] The invention belongs to the field of natural medicine chemistry and its quality control field, and relates to a method for measuring the weight-average molecular weight and content of polyguluronic acid sulfate. Background technique [0002] Sodium alginate is graded by acid hydrolysis to prepare polyguluronic acid, which is then sulfated to obtain polyguluronic acid sulfate, whose structure is 2-OH / 3-OH sulfuric acid It is a linear compound composed of degraded L-Guluronic acid (L-Guluronic acid, G) linked by α-1,4-glycosidic bonds. At present, there are domestic and foreign literature reports that polyguluronic acid sulfate can be used for the prevention and treatment of urolithiasis, and also has anti-tumor biological activity. [0003] [0004] Polyguluronic Acid Sulfate Structural Formula [0005] The weight-average molecular weight and content of polyguluronic acid sulfate are important determination parameters for the development of polygu...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 曾洋洋黄道林张真庆
Owner GREEN VALLEY (SHANGHAI) PHARM CO LTD
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