CN105806988A - Method for measuring content of glycine betaine in fructus lycii - Google Patents
Method for measuring content of glycine betaine in fructus lycii Download PDFInfo
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- CN105806988A CN105806988A CN201610147099.7A CN201610147099A CN105806988A CN 105806988 A CN105806988 A CN 105806988A CN 201610147099 A CN201610147099 A CN 201610147099A CN 105806988 A CN105806988 A CN 105806988A
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention discloses a method for measuring the content of glycine betaine in fructus lycii.At present, research on methods for measuring the content of glycine betaine in fructus lycii is increased; however, the methods have defects and disadvantages, the method for measuring the content of glycine betaine in fructus lycii overcomes defects of existing technologies and methods and is complete in extraction, easy and convenient to operate and capable of rapidly and accurately analyzing the content of glycine betaine in fructus lycii.The method mainly includes the steps that 1, a glycine betaine comparison product is extracted, methyl alcohol is added for dissolution, and a comparison product solution is obtained; 2, dried or fresh fructus lycii fruits are taken, a proper amount of liquid nitrogen is added to crush the fructus lycii fruits, methyl alcohol is added for supersonic extraction, and a ample solution is obtained; 3, measuring is conducted according to a high performance liquid chromatography-evaporation light scattering method, an octadecyl key and a silica gel packed column are adopted, the flowing phase is composed of methyl alcohol and water with the volume ratio of methyl alcohol to water being 20: 80, flow velocity is 1 ml/min, the drift tube temperature is 40 DEG C, the atomization temperature is 40 DEG C, the comparison product and the sample solution are taken and fed, and corresponding chromatograph charts are obtained; 4, the chromatograph charts and peak areas corresponding to the comparison product and the sample solution are recorded, the content of the glycine betaine is calculated in a quantitative mode with an external standard method, and the process is completed.
Description
Technical field
The present invention relates to the assay method of a kind of Betaine from Lycium barbarum L, belong to technical field of analysis and detection.
Background technology
Fructus Lycii (Lycium barbarum L.) is Solanaceae, the dry fruit of the perennial machaka of Lycium, is integration of edible and medicinal herbs
Functional Special plant resource, there is the multiple efficacies such as liver nourishing item, enhancing immunity, blood fat reducing, antioxidation, antitumor.
Fructus Lycii planting area spreads all over the areas such as Ningxia, Xinjiang, Hebei, Inner Mongol, Qinghai, Gansu, the genuinest with the produced Fructus Lycii in Ningxia.
Matrimony vine active composition mainly has three major types, and glycine betaine is one of them.Glycine betaine is a class quaternary ammonium salt compound, be FRUCTUS LYCII,
One of main alkaloid in leaf, handle, it plays the effect of methyl donor in vivo, have promotion lipid metabolism, anti-fatty liver,
Protection kidney, blood pressure lowering, mitigation stress, the multiple pharmacological effect such as appetite stimulator, stable vitamin.Further, since Radix Betae alkalization
Learning stable in properties and be difficult to artificially add, the content measuring it can be also that the preparation containing glycine betaine provides feasible quality control method.
The most increasing to the research of the assay method of beet alkali content in Fructus Lycii, mainly there are colorimetry, titrimetry, thin layer
Chromatographic scan method, high performance liquid chromatography etc..These methods are respectively arranged with its feature, and colorimetry needs to take off glycine betaine primary extract
Multiple steps such as color, the Reinecke salt sedimentation method, processing method is loaded down with trivial details, affects accuracy and the repeatability of measurement result；Titrimetry becomes
Basis is the lowest to be disturbed by pigment composition in sample, measures terminal and is difficult to judge；Separating effect and method during thin layer chromatography scanning analysis
Repeatability is affected bigger by chromatographic condition such as developing solvent etc..HPLC-DAD detection method measures the beet alkali content in Fructus Lycii, by
Without conjugated system in betaine structure, uv absorption is weak, needs to detect at wavelength 192nm, 195nm, and sensitivity is less
Preferable.At present about using the research of HPLC-ELSD method detection Betaine from Lycium barbarum L also there is no fairly perfect scheme.
Summary of the invention
It is an object of the invention to overcome the deficiency of art methods, it is provided that a kind of extraction is completely, easy and simple to handle, quick, accurate
The method really analyzing Betaine from Lycium barbarum L.
For reaching above-mentioned purpose, the technical scheme is that
The assay method of a kind of Betaine from Lycium barbarum L, it is characterised in that comprise the following steps:
A, take glycine betaine reference substance add methanol dissolve make reference substance solution；
B, take dried fruit of lycium barbarum or fresh fruit, add appropriate liquid nitrogen and pulverize, add methanol supersound extraction, obtain need testing solution；
C, foundation tablets by HPLC-ELSD, use octadecyl key and silica filler post, and flowing is mutually
Methanol: water (V: V, 20: 80), flow velocity 1ml/min, drift tube temperature 40 DEG C, atomization temperature 40 DEG C, takes reference substance and confession
Test sample solution sample introduction respectively, obtains corresponding chromatogram；
D, the record reference substance chromatogram corresponding with need testing solution and peak area, calculate containing of glycine betaine with quantified by external standard method
Amount, to obtain final product.
Further, the Fructus Lycii sample glycine betaine Extraction solvent described in described step b is methanol.
Further, the Fructus Lycii sample described in described step b and methanol solution mass volume ratio are 1: 250.
Further, in described step b, the supersound extraction time is 15min.
Further, in described step c, flow and use methanol mutually: water (V: V, 20: 80).
Compared with prior art, there is advantages that
1, use ultrasonic extraction, the cavitation effect of ultrasound wave can strengthening extraction, accelerate extraction process, and mild condition,
Power consumption is few.
2, Extraction solvent is methanol, and Objective extraction thing dissolubility in methanol is 55g/100g, and with other solvent phases
Ratio, the chromatographic peak peak shape that the sample that methanol as solvent extracts obtains through liquid phase analysis is best, without conditions of streaking.
3, compared with existing HPLC-DAD method, HPLC-ELSD method is easy and simple to handle, sample without carrying out deriving,
Purification etc. process, and experimentation cost is low, and rapidly and efficiently, sample separating degree is good, highly sensitive.
Detailed description of the invention
It is below the present invention preferably embodiment, the most therefore defines protection scope of the present invention.
The assay method of a kind of Betaine from Lycium barbarum L is characterized in that comprising the following steps:
A, take glycine betaine reference substance add methanol dissolve make reference substance solution；
B, take dried fruit of lycium barbarum or fresh fruit, add appropriate liquid nitrogen and pulverize, add methanol supersound extraction, obtain need testing solution；
C, foundation tablets by HPLC-ELSD, use octadecyl key and silica filler post, and flowing is mutually
Methanol: water (V: V, 20: 80), flow velocity 1ml/min, drift tube temperature 40 DEG C, atomization temperature 40 DEG C, takes reference substance and confession
Test sample solution sample introduction respectively, obtains corresponding chromatogram；
D, the record reference substance chromatogram corresponding with need testing solution and peak area, calculate containing of glycine betaine with quantified by external standard method
Amount, to obtain final product.
Embodiment 1:
Implementing the mensuration scheme of Betaine from Lycium barbarum L in the present invention, Fructus Lycii sample adds appropriate liquid nitrogen and pulverizes, precision weighing according to
Mass volume ratio is 1: 250 addition methanol supersound extraction 15min, and 0.22 μm filtering with microporous membrane uses octadecyl key and silicon
Glue filled column, flowing is methanol mutually: water (V: V, 20: 80), flow velocity 1ml/min, drift tube temperature 40 DEG C, vapo(u)rizing temperature
40 DEG C, sample introduction 10uL analyzes mensuration.
Embodiment 2:
Shown in embodiment 1, except that Extraction solvent is pure water and methanol-water, measurement result finds, Aqua pure extract sample
The chromatographic peak peak shape of product analysis is slightly trailed, and the chromatographic peak peak shape hangover that the sample analysis that methanol-water extracts obtains is serious.
The chromatogram of the present embodiment is as shown in Fig. 1, Fig. 2 and Fig. 3, and wherein Fig. 1 is methanol extraction sample chromatogram figure, chromatograph
Peak-to-peak shape is good；Fig. 2 is Aqua pure extract sample chromatogram figure, and chromatographic peak slightly holds in the palm tail；Fig. 3 is that methanol-water extracts sample chromatogram figure,
Chromatographic peak torr tail is serious.
Embodiment 3:
Shown in embodiment 1, except that extracting mode uses reflux, extract, carry it was found that supersound extraction relatively refluxes
Take in hgher efficiency.Different extracting mode gained extraction effect such as following tables:
The different extracting mode extraction effect of table 1 compares
Embodiment 4:
Shown in embodiment 1, except that the mass volume ratio extracting sample and solvent is 1: 125 and 1: 200, result
Find that solid-liquid ratio is reduced or increased extraction ratio and all reduces.Its different feed liquid is than the extraction effect such as following table of gained:
Table 2 different feed liquid compares extraction effect
Claims (5)
1. an assay method for Betaine from Lycium barbarum L, is characterized in that described assay method comprises the following steps:
A, take glycine betaine reference substance add methanol dissolve make reference substance solution；
B, take dried fruit of lycium barbarum or fresh fruit, add liquid nitrogen and pulverize, add methanol supersound extraction, obtain need testing solution；
C, foundation tablets by HPLC-ELSD, octadecyl key and the pillar of silica filler, flowing is methanol mutually:
Water (20: 80), flow velocity 1ml/min, drift tube temperature 40 DEG C, vapo(u)rizing temperature 40 DEG C, take reference substance and need testing solution difference
Sample introduction, obtains corresponding chromatogram；
D, the record reference substance chromatogram corresponding with need testing solution and peak area, calculate the content of glycine betaine, to obtain final product with quantified by external standard method.
The assay method of a kind of Betaine from Lycium barbarum L the most according to claim 1, is characterized in that the Chinese holly described in described step b
Qi sample glycine betaine Extraction solvent is methanol.
The assay method of a kind of Betaine from Lycium barbarum L the most according to claim 1, is characterized in that the Chinese holly described in described step b
Qi sample and methanol solution mass volume ratio are 1: 250.
The assay method of a kind of Betaine from Lycium barbarum L the most according to claim 1, is characterized in that supersound extraction in described step b
Time is 15min.
The assay method of a kind of Betaine from Lycium barbarum L the most according to claim 1, is characterized in that in described step c, and flow phase
Employing methanol: water (V: V, 20: 80).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108593798A (en) * | 2018-04-26 | 2018-09-28 | 中国科学院兰州化学物理研究所 | High performance liquid chromatography measures oil well and notes the method for adopting sulfobetaines surfactant content in liquid |
| CN110174366A (en) * | 2019-06-12 | 2019-08-27 | 酒泉市食品检验检测中心 | The extraction detection method of glycine betaine in a kind of fructus lycii |
| CN110376297A (en) * | 2019-06-13 | 2019-10-25 | 宁夏农林科学院枸杞工程技术研究所 | A kind of extraction and detection method of fructus lycii phenol amine substance asafoetide acyl agmatine |
| CN113698309A (en) * | 2021-09-10 | 2021-11-26 | 中南民族大学 | Method for extracting and separating betaine ester from bolete |
| CN113776907A (en) * | 2021-09-06 | 2021-12-10 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Method for extracting and detecting betaine in medlar |
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| CN103940931A (en) * | 2014-05-08 | 2014-07-23 | 山东省化工研究院 | Comprehensive quality evaluation method for betaine feed additive |
| RS20150353A1 (en) * | 2015-05-25 | 2015-12-31 | Nauäśni Institut Za Prehrambene Tehnologije | A new method for the extraction and quantitative determination of betaine in the cereals and pseudoceral products |
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2016
- 2016-03-05 CN CN201610147099.7A patent/CN105806988B/en not_active Expired - Fee Related
Patent Citations (2)
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| CN103940931A (en) * | 2014-05-08 | 2014-07-23 | 山东省化工研究院 | Comprehensive quality evaluation method for betaine feed additive |
| RS20150353A1 (en) * | 2015-05-25 | 2015-12-31 | Nauäśni Institut Za Prehrambene Tehnologije | A new method for the extraction and quantitative determination of betaine in the cereals and pseudoceral products |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108593798A (en) * | 2018-04-26 | 2018-09-28 | 中国科学院兰州化学物理研究所 | High performance liquid chromatography measures oil well and notes the method for adopting sulfobetaines surfactant content in liquid |
| CN110174366A (en) * | 2019-06-12 | 2019-08-27 | 酒泉市食品检验检测中心 | The extraction detection method of glycine betaine in a kind of fructus lycii |
| CN110376297A (en) * | 2019-06-13 | 2019-10-25 | 宁夏农林科学院枸杞工程技术研究所 | A kind of extraction and detection method of fructus lycii phenol amine substance asafoetide acyl agmatine |
| CN113776907A (en) * | 2021-09-06 | 2021-12-10 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Method for extracting and detecting betaine in medlar |
| CN113776907B (en) * | 2021-09-06 | 2023-11-14 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Extraction and detection method of betaine in medlar |
| CN113698309A (en) * | 2021-09-10 | 2021-11-26 | 中南民族大学 | Method for extracting and separating betaine ester from bolete |
| CN113698309B (en) * | 2021-09-10 | 2024-02-06 | 中南民族大学 | Method for extracting and separating betaine fat from bolete |
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