CN107315053A - About the EFI fog detector liquid phase chromatography analytical method of material in a kind of lactose - Google Patents
About the EFI fog detector liquid phase chromatography analytical method of material in a kind of lactose Download PDFInfo
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- CN107315053A CN107315053A CN201710400744.6A CN201710400744A CN107315053A CN 107315053 A CN107315053 A CN 107315053A CN 201710400744 A CN201710400744 A CN 201710400744A CN 107315053 A CN107315053 A CN 107315053A
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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
- G01N30/02—Column chromatography
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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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The invention provides the EFI fog detector liquid phase chromatography analytical method in a kind of lactose about material, chromatographic column is polymer nh 2 column, and acetonitrile water is mobile phase, the mL/min of flow velocity 1.0,30 DEG C of column temperature, EFI fog detector;This method can be analyzed simultaneously between galactolipin in lactose, glucose, lactulose, sucrose impurity, each impurity peaks and the separating degree between main peak and other impurities peak is all higher than 1.5, and calculating the theoretical number of plates with lactose chromatographic peak is more than 5000, and tailing factor is less than 1.2;The method sensitivity height, reappearance and good separating effect are easy to operate, quick, accurate, it is adaptable to lactose quality control and the research of relevant material.
Description
Technical field
The present invention relates to the quantitative detection in a kind of lactose about material, more particularly to the electricity in a kind of lactose about material
Spraying detector liquid phase chromatography analytical method.
Background technology
Lactose(lactose)It is naturally present in the reducing disaccharides in animal emulsion, human milk and contains in 5%~8%, cow's milk
Containing 4%~5%, (Fig. 1) is constituted by a molecule glucose and a molecule galactolipin, there are ɑ and β amphitypys.
ɑ type β types
In medical industry, available for the sweetener and excipient of medicine, need to can be made into crystalline lactose according to pharmaceutical formulation, straight
Press lactose and premix lactose auxiliary material.Lactose content and relevant material reflect product quality and nutritive value.Therefore, one is set up
Easy quick, sensitive and accurate analysis method, has important guidance to make for difference lactose quality and control Product Process etc.
With.
At present, it is many about the report of carbohydrate detection method both at home and abroad, it is roughly divided into two major classes:One class is enzymology side
Method, the method degree of accuracy and specificity are poor, while the source of enzyme is with purifying, there is also larger problem.Another kind of is chromatography, main
Will include gas chromatography (GC), Liquid Chromatography/Mass Spectrometry, chromatography of ions-Pulse amperometric detection method, liquid chromatogram differential detection method and
Liquid chromatogram evaporative light-scattering detector etc..Wherein, gas-chromatography and Liquid Chromatography/Mass Spectrometry need derivation process, cumbersome;From
Sub- chromatogram-pulsed amperometry method, instrument use cost is higher, and less stable, chromatographic condition is strict;Evaporative light-scattering is examined
Device liquid phase chromatography analytical method is surveyed, discovery is low there is also sensitivity, and poor reproducibility, the range of linearity is narrower, is also easy to produce baseline drift
The problems such as.Version in 2015《Chinese Pharmacopoeia》Middle lactose content and relevant substance-measuring use differential pulse polarograpll method, its spirit
Sensitivity is low, fluctuation affected by environment is larger, the problems such as unstability of base line, chromatographic peak profile are poor, chromatographic column service life is short easily occur.
Lactose molecule polarity is larger, does not have color functional group of Johnson & Johnson in structure, and UV absorption is weaker, it is impossible to using conventional anti-phase liquid
Phase chromatogram-UV-detector carries out accurate qualitative and quantitative measure.Consult the feelings that foreign latest standards of pharmacopoeia records lactose
Condition, it is found that only Europe and British Pharmacopoeia are controlled using gas chromatography to its content, and do not control relevant material.EFI
Fog detector is a kind of New-type detector developed in recent years, and the detector belongs to universal qualities type detector, and ultraviolet
Detector, differential refraction detector are compared with EISD, and sensitivity is high, and favorable reproducibility can be directly separated measure
The oligosaccharide such as monose and disaccharides.Have not yet to see using high performance liquid chromatography-EFI fog detector(HPLC-CAD)Method is surveyed simultaneously
Determine lactose content and the document report about material.
The content of the invention
The invention provides the EFI fog detector liquid phase chromatography analytical method in a kind of lactose about material, survey is established
Determine HPLC-CAD method of the lactose about material, new technological means is provided for the quality control of lactose.
About the EFI fog detector liquid phase chromatography analytical method of material in a kind of lactose, specific analytical method is as follows:
(1)Chromatographic condition is set:Polymer nh 2 column, acetonitrile-water is mobile phase, flow velocity 0.5-1.5 mL/min, column temperature 20-50
℃;EFI fog detector, detector atomization temperature:30-45 DEG C, power rate:1-1.2, sample frequency:10-15 Hz, filtering is normal
Number:3-4 s;
(2)It is prepared by system suitability solution:It is each suitable that precision weighs galactolipin, glucose, lactulose, sucrose and lactose control product
Amount, puts in 100mL measuring bottles, is well mixed, solubilizer dissolves and is diluted to scale, is used as system suitability solution;
(3)It is prepared by need testing solution:Milk sugar specimen about 100.0mg is taken, it is accurately weighed, put in 50 mL measuring bottles, add water appropriate, surpass
After sound, dissolving, scale is settled to acetonitrile, is shaken up, relevant substance-measuring need testing solution is used as;The need testing solution it is dense
Spend for 2.0 mg/mL;
(4)It is prepared by reference substance solution:Precision measures the mL of need testing solution 1.0, puts 100mL measuring bottles, and solubilization dilution agent is settled to quarter
Degree, is used as contrast solution;The concentration of the contrast solution is 20.0 μ g/mL;
(5)Detection:Precision is measured by step(2)The μ l of system suitability solution 20 of preparation, inject liquid chromatograph, each impurity
Separating degree between peak meets the requirements;Precision is measured by step again(4)The contrast solution of preparation and pass through step(3)Prepare
Each 20 μ l of need testing solution, are injected separately into liquid chromatograph, record chromatogram;
(6)According to the peak value in the chromatogram of need testing solution, calculated by Self-control method.
It is preferred that, the polymer nh 2 column is Shodex Asahipak NH2P-50 4E, 4.6 × 250 mm, 5 μm.
It is preferred that, the step(1)The proportioning of middle acetonitrile-water mobile phase is acetonitrile:Water=75:25.
It is preferred that, the step(2)Described in step(2)The concentration of middle lactose is 2.0mg/mL.
It is preferred that, defects inspecting is limited in the analysis method(S/N=3)For less than 10 ng, quantitative limit(S/N=10)It is less than
25 ng。
It is preferred that, the step(2)Middle solvent is acetonitrile.
This method can be additionally used in the detection of lactose content, and other contents of saccharide and about in the detection of material, such as
Sucrose, glucose, mannitol etc..
About the EFI fog detector liquid phase chromatography analytical method of material, specificity in a kind of lactose that the present invention is provided
By force, sensitivity is higher, and fluctuation affected by environment is smaller, and chromatographic peak profile is more excellent.Compared with the method that existing standards of pharmacopoeia is recorded,
Pharmacopeia method therefor is Composition distribution, and chromatographic system is stable to be needed at least 2 hours, and the present invention uses CAD detectors, chromatogram system
System is stable only to be needed 0.5 hour, shortens sample detection time;Other sample concentration is relatively low, and official method lactose concn is
100mg/mL, and lactose concn of the present invention only needs 2mg/mL, the amount into chromatographic column is smaller, extremely has to chromatographic column service life
Profit.
Brief description of the drawings
Fig. 1 is the chromatography figure of system suitability solution.
Embodiment
With reference to the accompanying drawings and detailed description, the present invention is furture elucidated.
Embodiment 1
Chromatographic condition:Chromatographic column is Shodex Asahipak NH2P-50 4E(4.6 × 250 mm, 5 μm)Mobile phase is second
Nitrile-water(75:25);The mL/min of flow velocity 1.0;20 DEG C of column temperature;EFI fog detector(Atomization temperature:30 ℃;Power rate:1;Sampling
Frequency:10 Hz;Filter constant:3s;Solvent:50% acetonitrile;The μ L of sample size 20.
The preparation of solution:
(1)System suitability solution
Appropriate known impurities reference substance (each impurity mass ratio is approximately equivalent to 0.5% principal component concentration) is added in milk sugar specimen,
The mixed solution of sample and impurity is made to investigate the specificity of method.
Precision weighs galactolipin, glucose, lactulose, sucrose and lactose control product in right amount respectively, puts in 100ml measuring bottles,
It is well mixed, plus acetonitrile dissolves and is diluted to scale, is used as system suitability solution;The chromatography figure of system suitability solution
As shown in Figure 1.
(2)Need testing solution
Milk sugar specimen about 100.0mg is taken, it is accurately weighed, put in 50 mL measuring bottles, add water appropriate, acetonitrile constant volume is used in ultrasound, dissolving
To scale, shake up, be used as relevant substance-measuring need testing solution(2.0 mg/mL).
(3)Contrast solution
Precision measures the mL of need testing solution 1.0, puts 100mL measuring bottles, and solubilization dilution agent is settled to scale, is used as contrast solution
(20.0 μg/mL).
Precision measures the μ l of system suitability solution 20, and the separating degree injected between liquid chromatograph, each impurity peaks should meet
It is required that;Precision measures contrast solution and each 20 μ l of need testing solution again, is injected separately into liquid chromatograph, record chromatogram to it is main into
Divide retention time 2 times.According to the peak value in the chromatogram of need testing solution, the amount about material is calculated by Self-control method.
Embodiment 2
Chromatographic condition:Chromatographic column is Shodex Asahipak NH2P-50 4E(4.6 × 250 mm, 5 μm)Mobile phase is second
Nitrile-water(75:25);Flow velocity 1.5mL/min;45 DEG C of column temperature;EFI fog detector(Atomization temperature:35 ℃;Power rate:1.15;Adopt
Sample frequency:12Hz;Filter constant:3.6 s;Solvent:50% acetonitrile;The μ L of sample size 20.
The preparation of solution:
(1)System suitability solution
Appropriate known impurities reference substance (each impurity mass ratio is approximately equivalent to 0.5% principal component concentration) is added in milk sugar specimen,
The mixed solution of sample and impurity is made to investigate the specificity of method.
Precision weighs galactolipin, glucose, lactulose, sucrose and lactose control product in right amount respectively, puts in 100ml measuring bottles,
It is well mixed, plus acetonitrile dissolves and is diluted to scale, is used as system suitability solution;The chromatography figure of system suitability solution
As shown in Figure 1.
(2)Need testing solution
Milk sugar specimen about 100.0mg is taken, it is accurately weighed, put in 50 mL measuring bottles, add water appropriate, acetonitrile constant volume is used in ultrasound, dissolving
To scale, shake up, be used as relevant substance-measuring need testing solution(2.0 mg/mL).
(3)Contrast solution
Precision measures the mL of need testing solution 1.0, puts 100mL measuring bottles, and solubilization dilution agent is settled to scale, is used as contrast solution
(20.0 μg/mL).
Precision measures the μ l of system suitability solution 20, and the separating degree injected between liquid chromatograph, each impurity peaks should meet
It is required that;Precision measures contrast solution and each 20 μ l of need testing solution again, is injected separately into liquid chromatograph, record chromatogram to it is main into
Divide retention time 2 times.According to the peak value in the chromatogram of need testing solution, the amount about material is calculated by Self-control method.
Embodiment 3
Chromatographic condition:Chromatographic column is Shodex Asahipak NH2P-50 4E(4.6 × 250 mm, 5 μm)Mobile phase is second
Nitrile-water(75:25);Flow velocity 0.5mL/min;50 DEG C of column temperature;EFI fog detector(Atomization temperature:45 ℃;Power rate:1.2;Sampling
Frequency:15 Hz;Filter constant:4 s;Solvent:50% acetonitrile;The μ L of sample size 20.
The preparation of solution:
(1)System suitability solution
Appropriate known impurities reference substance (each impurity mass ratio is approximately equivalent to 0.5% principal component concentration) is added in milk sugar specimen,
The mixed solution of sample and impurity is made to investigate the specificity of method.
Precision weighs galactolipin, glucose, lactulose, sucrose and lactose control product in right amount respectively, puts in 100ml measuring bottles,
It is well mixed, plus acetonitrile dissolves and is diluted to scale, is used as system suitability solution;The chromatography figure of system suitability solution
As shown in Figure 1.
(2)Need testing solution
Milk sugar specimen about 100.0mg is taken, it is accurately weighed, put in 50 mL measuring bottles, add water appropriate, acetonitrile constant volume is used in ultrasound, dissolving
To scale, shake up, be used as relevant substance-measuring need testing solution(2.0 mg/mL).
(3)Contrast solution
Precision measures the mL of need testing solution 1.0, puts 100mL measuring bottles, and solubilization dilution agent is settled to scale, is used as contrast solution
(20.0 μg/mL).
Precision measures the μ l of system suitability solution 20, and the separating degree injected between liquid chromatograph, each impurity peaks should meet
It is required that;Precision measures contrast solution and each 20 μ l of need testing solution again, is injected separately into liquid chromatograph, record chromatogram to it is main into
Divide retention time 2 times.According to the peak value in the chromatogram of need testing solution, the amount about material is calculated by Self-control method.
Above-described embodiment is only the preferred technical solution of the present invention, and is not construed as the limitation for the present invention, the present invention
The technical scheme that should be recorded with claim of protection domain, including in the technical scheme recorded of claim technical characteristic etc.
It is protection domain with alternative, i.e., equivalent substitution within this range is improved, also within protection scope of the present invention.
Claims (6)
1. about the EFI fog detector liquid phase chromatography analytical method of material in a kind of lactose, it is characterised in that concrete analysis side
Method is as follows:
(1)Chromatographic condition is set:Polymer nh 2 column, acetonitrile-water is mobile phase, flow velocity 0.5-1.5 mL/min, column temperature 20-50
℃;EFI fog detector, detector atomization temperature:30-45 DEG C, power rate:1-1.2, sample frequency:10-15 Hz, filtering is normal
Number:3-4 s;
(2)It is prepared by system suitability solution:Precision weighs galactolipin, glucose, lactulose, sucrose and lactose control product respectively
It is each appropriate, put in 100mL measuring bottles, be well mixed, solubilizer dissolves and is diluted to scale, is used as system suitability solution;
(3)It is prepared by need testing solution:Milk sugar specimen about 100.0mg is taken, it is accurately weighed, put in 50 mL measuring bottles, add water appropriate, surpass
After sound, dissolving, scale is settled to acetonitrile, is shaken up, relevant substance-measuring need testing solution is used as;The need testing solution it is dense
Spend for 2.0 mg/mL;
(4)It is prepared by reference substance solution:Precision measures the mL of need testing solution 1.0, puts 100mL measuring bottles, and solubilization dilution agent is settled to quarter
Degree, is used as contrast solution;The concentration of the contrast solution is 20.0 μ g/mL;
(5)Detection:Precision is measured by step(2)The μ l of system suitability solution 20 of preparation, inject liquid chromatograph, each impurity
Separating degree between peak meets the requirements;Precision is measured by step again(4)The contrast solution of preparation and pass through step(3)Prepare
Each 20 μ l of need testing solution, are injected separately into liquid chromatograph, record chromatogram;
(6)According to the peak value in the chromatogram of need testing solution, calculated by Self-control method.
2. according to claim 1 in a kind of lactose about material EFI fog detector liquid phase chromatography analytical method, it is special
Levy and be:The polymer nh 2 column is Shodex Asahipak NH2P-50 4E, 4.6 × 250 mm, 5 μm.
3. according to claim 1 in a kind of lactose about material EFI fog detector liquid phase chromatography analytical method, it is special
Levy and be:The step(1)The proportioning of middle acetonitrile-water mobile phase is acetonitrile:Water=75:25.
4. according to claim 1 in a kind of lactose about material EFI fog detector liquid phase chromatography analytical method, it is special
Levy and be:The step(2)The concentration of middle lactose is 2.0mg/mL.
5. according to claim 1 in a kind of lactose about material EFI fog detector liquid phase chromatography analytical method, it is special
Levy and be:Defects inspecting limit is less than 10 ng in the analysis method, and quantitative limit is less than 25 ng.
6. according to claim 1 in a kind of lactose about material EFI fog detector liquid phase chromatography analytical method, it is special
Levy and be:The step(2)Middle solvent is acetonitrile.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ES2728137A1 (en) * | 2018-04-20 | 2019-10-22 | Saborit Florenci Cutrina | Lactose detection kit and detection procedure by applying it (Machine-translation by Google Translate, not legally binding) |
CN113301974A (en) * | 2019-01-25 | 2021-08-24 | 瑞泽恩制药公司 | On-line chromatography and electrospray ionization mass spectrometer |
CN113834871A (en) * | 2021-09-18 | 2021-12-24 | 北京中医药大学 | Method for rapidly analyzing low-molecular-weight sugar based on paper spray mass spectrum and application thereof |
CN114839299A (en) * | 2022-06-14 | 2022-08-02 | 哈药集团技术中心 | Disaccharide compound analysis method |
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CN106706798A (en) * | 2017-02-10 | 2017-05-24 | 漳州傲农牧业科技有限公司 | Lactose content detection method |
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CN106706798A (en) * | 2017-02-10 | 2017-05-24 | 漳州傲农牧业科技有限公司 | Lactose content detection method |
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游正琴等: "HPLC-CAD法同时测定乳制品中糖类", 《中国乳品工业》 * |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ES2728137A1 (en) * | 2018-04-20 | 2019-10-22 | Saborit Florenci Cutrina | Lactose detection kit and detection procedure by applying it (Machine-translation by Google Translate, not legally binding) |
WO2019202193A1 (en) * | 2018-04-20 | 2019-10-24 | Cutrina Saborit Florenci | Kit for detecting lactose and detection method using same |
CN113301974A (en) * | 2019-01-25 | 2021-08-24 | 瑞泽恩制药公司 | On-line chromatography and electrospray ionization mass spectrometer |
CN113834871A (en) * | 2021-09-18 | 2021-12-24 | 北京中医药大学 | Method for rapidly analyzing low-molecular-weight sugar based on paper spray mass spectrum and application thereof |
CN113834871B (en) * | 2021-09-18 | 2024-05-28 | 北京中医药大学 | Method for rapidly analyzing low-molecular sugar based on paper spray mass spectrum and application thereof |
CN114839299A (en) * | 2022-06-14 | 2022-08-02 | 哈药集团技术中心 | Disaccharide compound analysis method |
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