CN108226352A - Application of the LHJ solubilizer in the quantitative determination of indissoluble food additives - Google Patents
Application of the LHJ solubilizer in the quantitative determination of indissoluble food additives Download PDFInfo
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- CN108226352A CN108226352A CN201611135704.5A CN201611135704A CN108226352A CN 108226352 A CN108226352 A CN 108226352A CN 201611135704 A CN201611135704 A CN 201611135704A CN 108226352 A CN108226352 A CN 108226352A
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- G—PHYSICS
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- 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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- 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
LHJ solubilizer is made of enzyme, coenzyme, butanediol, benzalkonium chloride；It is mainly used for hygienic physical and chemical inspection field；Solve former national standard《Food sanitary testing method, physics and chemistry part》, problem very low to the indissoluble foodstuff synthetic additive quantitative determination rate of recovery.Without LHJ recovery of standard addition 30% 60%；With LHJ recovery of standard addition 90% 110%, meet Instrumental Analysis requirement；LHJ can be additionally used in additive, food in drug, feed, cosmetics and be forbidden to use the quantitative determinations such as object, pesticide residue, residue of veterinary drug.Technical solution：Indissoluble foodstuff is crushed, is put into water or mobile phase, adds in a certain amount of LHJ, big organic compound is digested solubilising stripping, additive is made to be exposed in aqueous solution by LHJ, then centrifugal filtration is quantitative determined in high performance liquid chromatography, gas chromatograph.LHJ will adhere to the stripping dissolving of chromatographic column hydrophobe, shorten washing time, can make chromatographic column eluant, eluent.
Description
Technical field：The present invention relates to indissoluble foodstuff health physical and chemical inspection fields；It is Specifically LHJ enzymes-coenzyme, non-
For cationic surfactant by the big organic molecule enzymolysis of indissoluble foodstuff into small molecule, non-cationic surfactant reduces water
Surface tension by colloid-suspension particles stripping dispersion, makes additive be substantially dissolved in water phase, solves former national standard method, difficult
Dissolve the very low problem of the food additives quantitative determination rate of recovery.
Background technology：I is engaged in high performance liquid chromatography work for many years, finds<<National Standard of the People's Republic of China eats
Product sanitary inspection method (one) P1-709, (two) P1-596Fluid sample (such as carbonated drink, beverage, assembled alcoholic drinks) is only adapted to, to solid-half
Preservative, sweetener, pigment, brightening agent etc. in solid food, such as jelly, dried orange peel, jam, preserved fruit, cake food, it is quantitative to survey
Determine the rate of recovery (30%-60%), can not Accurate Determining additive real content, exceeded food can not strictly be controlled to flow into city
！It is very unfavorable to people's health, special carcinogenic substance！The work that studies for a long period of time is carried out thus, it is difficult with water or flowing phased soln
Food is dissolved, there are many colloid-suspended substances, and intermolecular (Van der Waals force, the hydrogen bond, cohesive energy) gravitation of blob of viscose-suspended substance is very big, special
Other cohesive energy is not also reduced with protein precipitant-ultrasound, additive is firmly adsorbed to capsule and is wrapped up in！One kind is had been look for for many years
Reagent eliminates suspended substance gravitation-stripping dispersion suspended substance granularity, additive is extracted to come from suspended substance, fully exposure dissolving
In water phase；It when later son eats jelly, is dropped on jelly with asparagus juice, as a result, jelly dissolves a hole！Me has been reminded under this,
Start thus up to several years LHJ extractions mixture-application study work, LHJ researchs are used successfully to benzoic acid in indissoluble foodstuff, mountain
In potassium sorbate, saccharin sodium, benzoyl peroxide quantitative determination,《LHJ solubilizer is used for benzoic acid and sorbic acid in jelly and quantitatively surveys
Fixed research》, paper publication<<Chinese Journal of Health Laboratory Technology>>2004.12.14 roll up 6 phase P713-714, it is second-class to obtain city's scientific and technological progress
Prize.《Benzoic acid, sorbic acid, saccharin sodium LHJ solubilising high performance liquid chromatographies in dark, indissoluble food》Publication exists《Occupation
With health》23 phases of volume 25 in 2009；《The Reduction by Thiosulfate LHJ solubilising high performance liquid chromatography of benzoyl peroxide in flour
Measuring method》Publication was 24 phases of volume 25 in 2009, and for several method recovery of standard addition between 90%-110%, meeting Instrumental Analysis will
It asks.《LHJ solubilizer in slightly solubility food additive quantitative determine study, efficient night phase color method》, obtain city's science and technology into
Walk second prize (2013)；Other additive method for quantitatively determining are just under study for action.
Invention content：Difficult food is crushed, weighs 1.0-2.5 grams of sample, 10.0-25.0 milliliters of colorimetric cylinders is put into, adds
5.0-10.0 milliliters of mobile phases, shaking, add LHJ2.0-5.0ml shake wells, put 30min, add in 200g/L zinc acetates and
100g/L potassium ferrocyanides each 0.5ml or 2.5mL, shake well add mobile phase constant volume to shake up to 10.0mL-25.0mL scales,
Centrifugation, takes supernatant to cross 0.45um filter membranes, and 10.0uL sample solutions and standard solution is taken to inject high performance liquid chromatograph and determined
It is fixed to measure.
High performance liquid chromatography uses reversed post separation, ultraviolet or diode assessor quantitative determination additive real content；
Key is LHJ and contains plant-animal glue, albumen, fat, carbohydrate, thickener etc., and enzymolysis-solubilising-stripping makes suspension
Body minimization of particle size！Additive fully exposure dissolving water phase, then centrifuge, cross miillpore filter, upper high performance liquid chromatography quantitative determination.
The application that preservative quantitative determines in indissoluble food of embodiment 1, LHJ solubilizer：
(description of the drawings：Attached drawing 1 is with being compared without LHJ to benzoic acid, sorbic acid quantified results in jelly) food
Savor 28 kinds of preservative；To containing (such as jelly, dried orange peel, sauce class, the honey such as plant-animal glue, albumen, fat, carbohydrate, thickener
Candied fruit, soft sweets, jam, meat, egg, fish, poultry product, collagen sugar-coat, jam cake and bread, cake, moon cake) etc., benzoic acid, mountain
Pears acid quantitative determines, and before LHJ useless, jelly recovery of standard addition only has 30%, when with LHJ, colloid completely disappears, benzene first
Acid, sorbic acid are dissolved completely in water phase, and recovery of standard addition benzoic acid 90.7%, potassium sorbate 96.7% comply fully with instrument
Analysis requirement, paper publication exist《Chinese Journal of Health Laboratory Technology》2004th, 12,14,6 phase P713-714, 2005, obtain section of city progress two
Deng prize.
The application that sweetener quantitative determines in indissoluble foodstuff of embodiment 2-1, LHJ solubilizer：
(description of the drawings：Attached drawing 2 be with without LHJ to benzoic acid, sorbic acid, saccharin quantitative determination of sodium in indissoluble food
Comparative result)；GB 2760-2013, sweetener have it is ten several, it is common to have saccharin sodium, honey element, acesulfame-K, alitame, A Si
Ba Tian, neotame etc.；Sample treatment：Food such as (plant-animal glue, albumen, fat, carbohydrate, thickeners) will be contained, such as honey
Candied fruit, ice cream, ice river in Henan Province class can, jam etc., which are smashed to pieces, is put into water or mobile phase, and there are many colloid-suspended substances to occur！Have to sweetener
Very absorption capsule wraps up in effect by force, causes the quantitative determination rate of recovery 40% or so；The dissolving of sweetener is substantially increased with LHJ
Degree；Principle is same as Example 1, paper《Dark, benzoic acid, sorbic acid, saccharin sodium in indissoluble food the efficient liquid of LHJ solubilisings
Phase chromatographic detection》Publication exists《Occupation and health》23 phases of volume 25 in 2009, recovery of standard addition benzoic acid 90%-108%, sorb
Sour 90%-100%, saccharin sodium 90%；Technical indicator all meets Instrumental Analysis requirement.
The application that sweetener (honey element) quantitative determines in indissoluble foodstuff of embodiment 2-2, LHJ solubilizer：
Jelly sample is broken, it is put into test tube, adds a small amount of water dissolution, LHJ shake wells is added to dissolve constant volume, be situated between in acidity
Honey element generates cyclohexanol nitrous acid ester with nitrite reaction in matter, is extracted with n-hexane, gas-chromatography separation, and retention time is fixed
Property, quantified by external standard method；As a result this method linear relationship in 0.25-10 nanogram ranges is good, related coefficient 0.9996, detection
It is limited to 0.001g/kg, rate of recovery 90%-102%；Conclusion, this method sensitivity-precision is good, and the rate of recovery is high, with LHJ processing
Sample honey element measurement result improves 2-3 times；Paper《The application that LHJ solubilizer quantitative determines honey element in jelly》Publication exists
《The anti-system of medical faunae》08 phase in 2015.
The application of embodiment 3, LHJ solubilizer in brightening agent quantitative determination：
(description of the drawings：Attached drawing 3 is with being compared without benzoyl peroxide quantified results in LHJ flour) brightening agent
There are many, benzoyl peroxide belongs to food and is forbidden to use object, because resolving into benzoic acid in human body, there is carcinogenesis！It can be illegal
Molecule is always using, so research accurate quantitative analysis method is necessary；Have document announcement, with ethyl alcohol dissolving again with iodate nak response
Benzoic acid is generated, because ethyl alcohol and potassium iodide addition are too big, baseline non-return-to-zero, solvent peak extra wide is decomposed with benzoyl peroxide and produced
Object benzoic acid peak is inseparable, can not Accurate Determining benzoic acid real content, ethyl alcohol and the very little benzoyl peroxide first of potassium iodide addition
Decompose incomplete, also macromolecular para Toluic Acid adsorbs capsule and wraps up in effect, caused by several factors！Determination of benzoyl peroxide in wheat is neglected height and is neglected
It is low, true value can not be measured.Using Reduction by Thiosulfate, LHJ enzymolysis-solubilising-stripping is eliminated suspended substance para Toluic Acid and is adsorbed and makees
With, make benzoic acid fully exposure be dissolved in water phase, solvent peak narrows, benzoic acid in the case that baseline be zeroed ability appearance, finally build
Vertical benzoyl peroxide accurate quantitative analysis method,《The sodium thiosulfate of benzoyl peroxide also LHJ solubilisings high-efficient liquid phase color in flour
Compose measuring method》Recovery of standard addition 92.0%, technical indicator meet Instrumental Analysis requirement.
The quantitative application of colorant in indissoluble food of embodiment 4, LHJ solubilizer：
GB2760-2013 colorants have tens kinds, and secondary colour is known as seven kinds of (Jian Caihong, famille rose, red scarlet, newly red, lemons
It is lemon Huang, sunset yellow, brilliant blue, indigo), there are candy, cake, green plum, Hawthorn containing dynamic-natural plant gum and thickener indissoluble foodstuff
Product, red and green pickled fruit, marasca can, bologna sausage casing, ice cream, tartar sauce, jelly watermelon jam can, candy, ice cream, biscuit
There is colloid-suspended substance to have the absorption capsule property wrapped up in pigment in course of dissolution Deng, these food, pigment cannot be dissolved in water, fixed
It is very low that the rate of recovery is determined in measurement, in addition between LHJ rate of recovery 90%-110%, meets Instrumental Analysis requirement.
Embodiment 5, pigment, which are surveyed, damages seriously performance liquid chromatographic column, and a pigment detection, the same day does not rush pillar
Wash clean rinses, on color adherent pillar, how also not to be washed clean with water-methanol, swept away soon perhaps with LHJ later for second day
More substances, tonsure elute 3 pillars and have rinsed；It is that pillar rinses that high performance liquid chromatography, which measures key, many organic-inorganics
It is attached on pillar, is needed to rinse for a long time with mobile phase or methanol, with LHJ wash cleans quickly, application method, in injection port
LH injection J repeatedly.
Embodiment 6, LHJ are that tool enzymolysis-solubilising-stripping is integrated chemical reagent in indissoluble enzymatic hydrolysis system, can solve national standard side
Method quantitative determines the low-down problem of the rate of recovery to indissoluble foodstuff additive.
Claims (6)
1.LHJ solubilizer it is characterized in that：LHJ is made of aloe enzyme-coenzyme, butanediol, benzalkonium chloride；Major function is
Enzyme-coenzyme digests the macromoleculars such as dynamic-natural plant gum, albumen, fat, polysaccharide, fiber, thickener；Non- cationic surfactant
Water phase surface tension is reduced, stripping dispersion suspended substance granularity makes additive fully exposure be dissolved in water phase；Before LHJ useless,
Indissoluble foodstuff discharges water middle shake well, and solution exists with colloid-suspended substance, solid phase gravitation (cohesive energy, hydrogen bond, Van der Waals force)
It is very big, firmly additive absorption capsule is wrapped up in, additive, which cannot expose, to be dissolved in water phase, causes additive quantitative determination recycling
Rate 30%-60%；Big organic molecule is digested when adding in LHJ solubilizer, non-cationic surfactant hydrophilic group is formed with water
A hydrogen bond increases solubility in water, and hydrophilic group becomes meander configuration from sawtooth pattern, and hydrophilic oxygen is located on the outside of chain, and hydrophobic group-
CH2-Base is located on the inside of chain, thus surrounding becomes easily to be combined with water, while cationic surfactant plays stripping dispersion work(
Can, make suspended substance minimization of particle size, additive fully exposure is dissolved in water phase；Centrifugation-too small miillpore filter, sample solution are presented
Water white transparency state, high performance liquid chromatography quantitative determination, the rate of recovery is between 90%-110%；LHJ be additionally operable to (feed, drug,
Daily necessities, makeup) in additive, food be forbidden to use object, pesticide residue, the quantitative determination of residue of veterinary drug.
2. according to claim 1 told with LHJ it is characterized in that, LHJ can will contain-natural plant gum, albumen, fat, carbon aquation
The macromoleculars such as object, thickener, antioxidant enzymolysis is closed into small molecule；Non- cationic surfactant reduces water surface tension, stripping
From dispersion suspended substance granularity, additive fully exposure is made to be dissolved in water phase；Easy to operate, quick, sample treatment is in a container
It carries out, reduces systematic error, improve the additive quantitative determination rate of recovery；What is indissoluble foodGeneral solid, semisolid
Food belongs to indissoluble foodstuff！It is crushed and is put into water phase, existed with colloid-suspension form；Additive quantitative determines back
Yield 30%-60%；It all needs to digest-solubilising-stripping with LHJ；Miillpore filter-upper instrument quantitative is centrifuged-crosses again to measure.This is this
The main contents of patent protection；LHJ is additionally operable to additive, food in (feed, drug, daily necessities, makeup) and (is forbidden to use
Object, pesticide residue, residue of veterinary drug) quantitative determination.
3. contain the indissolubles food such as dynamic-natural plant gum, albumen, fat, carbohydrate, thickener according to what claim 2 was told,
- solubilising-stripping need to be digested with LHJ, what food is containing dynamic-natural plant gum, albumen, fat, carbohydrate, thickener
Such as jelly, ice cream, ice cream, cake, biscuit, instant coffee, chocolate, bread, dairy products, meat products, jam, Seasoning Paste
Juice, shortening dilated food, fish product, chewing gum, noodles, fruit juice, condensed milk, hydrogenated vegetable oil sauce, vegetable protein beverage, sauce
Class, cereal product, preserved fruit etc. belong to indissoluble food；- solubilising-stripping, centrifugation-mistake miillpore filter-upper height need to be digested with LHJ
Effect liquid phase chromatogram measures.This is this patent protection main contents.LHJ is additionally operable to add in (feed, drug, daily necessities, makeup)
Add agent, food (being forbidden to use object, pesticide residue, residue of veterinary drug) quantitative determination.
4. being told according to claim 3, indissoluble food additives measure need to digest-solubilising-stripping with LHJ, then efficient night phase
Chromatogram quantification measures；Food additives have preservative, sweetener, brightening agent, colorant, acidity agent, anticaking agent, antioxidant,
Emulsifier etc., is shown in GB2760-2011.The basic method of inspection《National Standard of the People's Republic of China's food sanitary testing method
(1) P1-700, (two) P1-596>；Indissoluble food additives measure, on the basis of National Standard Method is used, with LHJ sample pre-treatments, then on
High performance liquid chromatography measures, and has example at present, and the rate of recovery meets Instrumental Analysis requirement between 90%-110%；It is other
Just under study for action, this is this patent protection main contents to method for quantitatively determining；LHJ is additionally operable to (feed, drug, daily necessities, makeup
Product) in additive, food (being forbidden to use object, pesticide residue, residue of veterinary drug) quantitative determination.
5. it is told with LHJ according to claim 2 it is characterized in that, it can digest macromolecular into small molecule, non-cationic surface
Activating agent reduces bur on water surface tension-stripping dispersion pillar, into mobile phase, shortens pillar washing time, can conduct
Performance liquid chromatographic column eluant, eluent；This is the content of this patent protection.
6.LHJ is in indissoluble system, it is that have the chemical reagent that enzymolysis-solubilising-stripping is integrated, to solve indissoluble food additives
Quantitative determine the low problem of the rate of recovery.
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| CN201611135704.5A CN108226352A (en) | 2016-12-12 | 2016-12-12 | Application of the LHJ solubilizer in the quantitative determination of indissoluble food additives |
| CN202111141237.8A CN113866327A (en) | 2016-12-12 | 2016-12-12 | Application of LHJ solubilizer in quantitative determination of insoluble food additives |
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