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Method for measuring saccharide content in fragrant solomonseal rhizome by adopting GC-MS method

A GC-MS, Polygonatum japonica technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of poor reproducibility, difficult control, single quality control indicators, etc., and achieve strong controllability and measurement accuracy. High precision and clear measurement indicators

Inactive Publication Date: 2015-12-02
HUNAN UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Polygonatum Polygonatum mainly contains polysaccharides with relatively large molecular weight and many hydroxyl groups. The index of quality control is total polysaccharides. At present, the ultraviolet-visible spectrophotometry method is used. This method has large errors, single quality control indicators, and poor reproducibility. Good, difficult to control, affecting the formulation of its quality standards and the quality control of raw medicinal materials and Chinese patent medicines

Method used

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  • Method for measuring saccharide content in fragrant solomonseal rhizome by adopting GC-MS method
  • Method for measuring saccharide content in fragrant solomonseal rhizome by adopting GC-MS method
  • Method for measuring saccharide content in fragrant solomonseal rhizome by adopting GC-MS method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1 adopts GC-MS method to analyze carbohydrate TMS derivative in Polygonatum Polygonatum

[0032] 1. Sample processing: Polygonatum odoratum Xiang, Jiangbei Polygonatum, and Guan Yuzhu were used as test objects, and Polygonatum odoratum powder was prepared respectively. Precisely weigh 0.05g Polygonatum odoratum powder, add 1ml DMF and 0.ml silanization reagent to a 2ml chromatographic sample bottle, cover the bottle tightly and shake well, put it in an oven at about 70°C for about 20-30min, then cool to room temperature , using GC-MS method for injection analysis.

[0033] 2. GC-MS detection: Gas chromatography conditions are: chromatographic column: capillary column Rtx-5ms with specifications of 30m×0.25mm×0.25μm; carrier gas: He; flow rate: 1.0mL / min; inlet temperature: 250 ℃; temperature program: initial temperature 60 ℃, keep 1min, raise temperature to 100℃ at 5℃ / min, keep 2min, then raise temperature to 220℃ at 3℃ / min, keep 5min, then raise temperature...

Embodiment 2

[0039] The optimization of the extraction method of sucrose and glucose TMS derivatives in Polygonatum Polygonatum in embodiment 2

[0040] The contents of sucrose and glucose measured by internal standard method were used as indexes for the evaluation and selection of each level and factor, and the orthogonal experiment design is shown in Table 2.

[0041] Table 2 Orthogonal design table for the extraction method of Polygonatum odoratum TMS derivatives

[0042]

[0043] Accurately weigh about 0.05 g of Polygonatum odoratum powder, carry out the experiment according to Table 3, pass through a 0.45 μm microporous membrane, set the volume to 2 ml, shake well, and carry out sample detection according to the method in Example 2. Orthogonal experiment results are shown in Table 3.

[0044] Form 3L 9 (3 4 ) Orthogonal experimental results

[0045]

[0046] According to the analysis of variance of the orthogonal experiment, the optimal extraction parameter is selected as A 2...

Embodiment 3

[0047] Embodiment 3 Polygonatum odoratum dry powder and the screening of conditions

[0048] 1. Dry powder of Polygonatum odoratum (coarse powder, coarse powder, medium powder, fine powder, finest powder and very fine powder) and drying conditions (shade drying method, vacuum drying method, drying method and traditional sugar kneading method) according to The best extraction parameters and control indicators provided in Example 3 were tested, and a one-way analysis of variance was carried out. The results are shown in Table 4 (P<0.005), indicating that there are differences among various powders.

[0049] Table 4 Results of variance analysis of Polygonatum odoratum dry powder with different fineness

[0050]

[0051] 2. Using LSD method and Dunnett method for multiple comparisons, coarse powder, medium powder, fine powder, the finest powder and very fine powder are compared with the coarsest powder respectively, and Polygonatum fine powder has a higher total content than ot...

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Abstract

The invention provides a method for measuring saccharide content in fragrant solomonseal rhizome by adopting a GC-MS method. The method comprises the steps of processing fragrant solomonseal rhizome to be powder, then drying the powder, adding DMF and a silanization reagent into the fragrant solomonseal rhizome powder, reacting under a certain condition, carrying out derivatization on the saccharides in the fragrant solomonseal rhizome to form saccharide TMS derivatives, and then measuring the content of the saccharide TMS derivatives in the fragrant solomonseal rhizome by adopting the GC-MS method, thus measuring the saccharide content in the fragrant solomonseal rhizome. According to the method, silyl is introduced into saccharide molecules by utilizing the silanization reagent, so that the polarity of a saccharide compound is reduced, the composition of the saccharide TMS derivatives of the fragrant solomonseal rhizome can be analyzed by adopting the GC-MS internal standard method, the measuring accuracy and the measuring precision of the content of saccharose and glucose are high, the measurement index is accurate, the controllability is strong, and the new method is provided for optimization and upgrading of a quality evaluation criterion system of the fragrant solomonseal rhizome.

Description

technical field [0001] The invention relates to the formulation of quality standards for traditional Chinese medicinal materials, and relates to a method for measuring sugar content in Polygonatum Polygonatum by using a GC-MS method. Background technique [0002] Yuzhu is the dry rhizome of Polygonatumodoratum (Mill.) Druce, a plant belonging to the genus Polygonatum in the Liliaceae family (Liliaceae). As a common Chinese medicinal material for both medicine and food, it has a long history and has a long-standing reputation at home and abroad. As early as in "Shen Nong's Materia Medica", it is recorded that Polygonatum odoratum is sweet and flat; it has the effects of nourishing yin and moistening dryness, promoting body fluid and quenching thirst. Treatment of febrile diseases and yin injuries, cough and polydipsia, fever due to consumptive fatigue, hunger due to Xiaogu, frequent urination and other diseases. Polygonatum Polygonatum contains a variety of chemical substan...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 刘塔斯刘应蛟曾晓艳龚力民
Owner HUNAN UNIV OF CHINESE MEDICINE
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