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Dried ginger quality evaluation method based on UPLC-TQ-MS/MS

A UPLC-TQ-MS and quality evaluation technology, which is applied in the field of quality analysis of traditional Chinese medicine, can solve the problems of single quantitative component type, long time for quality analysis of dried ginger, inability to effectively distinguish dried ginger and sulfur-smoked dried ginger, and achieve specificity Strong, guaranteed safety and effectiveness

Active Publication Date: 2022-03-22
JINAN UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the technical problems that the quality analysis time of dried ginger in the existing liquid mass spectrometry technology is long, the type of quantitative components is single, and it is impossible to effectively distinguish dried ginger and sulfur-smoked dried ginger, thereby providing a method based on UPLC-TQ-MS / MS dry ginger quality evaluation method, the evaluation method can quickly distinguish between sulfur smoked and non-sulfur smoked dried ginger, and at the same time quantitatively evaluate the quality level of dried ginger, which is highly specific, accurate and reliable

Method used

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  • Dried ginger quality evaluation method based on UPLC-TQ-MS/MS
  • Dried ginger quality evaluation method based on UPLC-TQ-MS/MS
  • Dried ginger quality evaluation method based on UPLC-TQ-MS/MS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Treatment of Samples

[0033] 1, preparation of sample solution

[0034] Precisely weigh 0.1 g of dry ginger sample, extract 30 min with 10 ml 70% methanol (V / V), extract 13225 g from 10 min, to obtain a supernatant, diluted with 70% methanol (V / V) 100 μg / ml.

[0035] 2. Preparation of the standard solution of reference

[0036] Separating 6-gingerol, 6-gingerol, 6-dehydrogenol, 8-gingerol, 8-ginger, 8-dehydrotanol, 8-ginger, 8-dehydrogenol, 10 Ginger, 10-ginger, 10-dehydrotanculid, and spectroscopy of nuclear magnetic and high resolution mass spectrometry, the peak area is collected by the peak area, and the purity is higher than 98%.

[0037] 6-gingerol (160 mg) was dissolved in MeOH / PHME solution (4.5 mL / 1.5 ml), and add catalyst at 0 ° C (C 29 Hide 30 N 4O Fly 6 S, CAS: 852913-19-0, 35 mg, 0.1 equivalents) and NAHSO 3Aqueous solution (0.5m, 72 mg). After stirring at 0 ° C for 48 hours, the reaction was stopped and dried, then dissolved in methanol, f...

Embodiment 2

[0039] Example 2 Chromatography Condition Optimization

[0040] UPLC analysis is carried out on the ACQUITY UPLC 1-Class system equipped with a binary solvent system. Chromatography separation was achieved under 40 ° C column temperature conditions using a BEH SHIELD RP18 column. The mobile phase consists of water (a) and acetonitrile (B), both comprising 0.1% formic acid (V / V), gradient elution at a flow rate of 0.4 ml / min, and the injection volume was set to 2 μL.

[0041] By examining different elution procedures, the gradient elution process that can make the compound has better separation and better peak time as follows: 5% B, 0-0.5 min; 5-80% B, 0.5-10 min 80-100% B, 10-12 min; 100% B, 12-13 min, 100-5% B, 13-14 min; 5% B, 14-15 min.

[0042] The UPLC system and the triple quadrupole mass spectrometer are: using an electrospray ion source (ESL), a capillary voltage 2 kV, a tapered pore voltage 20 V, a dehydric gas temperature of 250 ° C, cone The pore gas flow rate is 15...

Embodiment 3

[0044] Example 3 Construction of Quantitative Analysis Method

[0045] 1, specialty test

[0046] The dry ginger sample solution obtained by Example 1 was applied, and the standard solution and blank solvent were performed, and UPLC-TQ-MS / MS measurement analysis was performed in accordance with the chromatographic conditions in Example 2. Figure 2-8 Indicated. Among them, A, B, and C represent dry ginger samples, standard solutions, and white solvents. 6GS, 6G, 6S, 6D, 8G, 8S, 8D, 10G, 10S and 10D represent 6-gumullic acid (retention time = 6.5 min), 6-gingerol (retention time = 6.5 min), 6-ginger Phenol (retention time = 7.8 min), 6-dehydrogenin (retention time = 8.7 min), 8-gingerol (retention time = 7.6 min), 8-gingerol (retention time = 8.9 min), 8 - Dehydrotionin (retention time = 9.6 min), 10-gingerol (retention time = 8.6 min), 10-gingerol (retention time = 9.8 min) and 10-dehydrotanolidone (retention time = 10.5 min).

[0047] According to this result, the sample matrix ...

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Abstract

The invention relates to a dried ginger quality evaluation method based on UPLC-TQ-MS / MS. According to the invention, the difference mark component 6-gingesulfonic acid before and after dry ginger smoking is compared with nine compounds (6-gingerol, 6-shogaol, 6-dehydrozingiberendione, 8-gingerol, 8-shogaol, 8-dehydrozingiberendione, 10-gingerol and 10-shogaol) which are mainly contained in other dry ginger, have remarkable biological activity and cover multiple types of structures; meanwhile, a UPLC-TQ-MS / MS mass analysis method is constructed, so that the stoving dried ginger and the non-stoving dried ginger can be quickly distinguished by one analysis method, and meanwhile, the quality level of the dried ginger is quantitatively evaluated. The method is high in specificity, accurate and reliable, provides technical support for safe use and stable quality of dried ginger, and provides a referential research method for quality evaluation of traditional Chinese medicinal materials / stoving traditional Chinese medicinal materials.

Description

Technical field [0001] The present invention belongs to the field of traditional Chinese medicine quality analysis, and specific relates to a dry ginger quality evaluation method based on UPLC-TQ-MS / MS. Background technique [0002] As a common Chinese herbal medicine, dry ginger is the dry roots of Jiangke Jiang's perennial plant ginger. As the first batch of Chinese herbal medicines listed in the country "in accordance with the traditional Chinese herbal medicine material catalog, dry ginger is the most useful history. One of the most widely used "medicinal food homologous" Chinese medicine; in terms of oxidative stress, inflammation, tumor, diabetes and gastrointestinal diseases show significant effects, with important medical and diet health care; It is also important economic plants, covers vast and widely circulated in China. [0003] However, reports of sulfur and sulfur ginger in the market in recent years are uncommon, and a series of studies have found that sulfur fum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/72
CPCG01N30/02G01N30/06G01N30/54G01N30/72Y02P90/30
Inventor 何亮亮陈沅姗孔紫璐李旭冰张梓若杨可枫陈歆彤姚志红
Owner JINAN UNIVERSITY
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