CN103675114A - Method for detecting erythritol - Google Patents
Method for detecting erythritol Download PDFInfo
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- CN103675114A CN103675114A CN201210360900.8A CN201210360900A CN103675114A CN 103675114 A CN103675114 A CN 103675114A CN 201210360900 A CN201210360900 A CN 201210360900A CN 103675114 A CN103675114 A CN 103675114A
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- antierythrite
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- erythritol
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Abstract
Erythritol is a white crystalline tetra-carbon polyol compound and a novel fermentation type low-calorie sweetener, and has wide application prospect in the fields such as medicine, food, cosmetics, and chemical industry; the study on the erythritol becomes a high-profile hot spot internationally at present. The invention provides a method for quantitative detection of the erythritol by ion chromatography; due to the method, the recovery rate reaches 85-90%; compared with the existing gas chromatographic method, a high performance liquid chromatography, a capillary electrophoresis method, the method has the advantages of high accuracy, no derivation, simplicity and convenience in operate, high sensitivity, environmental protection, good reproducibility and the like, thus being a practical detection method.
Description
One, technical field
The invention belongs to chemical analysis field, particularly use the technology of sulfate by ion chromatography antierythrite.
Two, background technology
Antierythrite chemical name Erythritol, English name Erythritol, molecular formula is C
4h
10o
4, molecular weight is 122.12, chemical structural formula as shown in Figure 1,126 ℃ of fusing points, boiling point 329-331 ℃, is a kind of four carbon polyols, outward appearance is white powdery crystallization, has refrigerant sense, thermal value is low, easily crystallization.
Antierythrite is four carbon polyol compounds of white crystals, it is a kind of novel fermentation type low calorie sweetener that adopts biotechnology to produce, in June, the 1999 international food adjuvant Committee of Experts (JECFA) ratifies antierythrite as edible sweetener, and without regulation ADI value.At present, antierythrite in states such as the U.S., Japan, New Zealand, Australia, Singapore, Korea S, Mexico for food production.In June, 2007 19 China Ministry of Public Health bulletin approval antierythrite is applied in the food such as chewing gum, solid beverage, modulation breast as sweetener.This novel sugar alcohol based food of antierythrite sweetener, has that heat is low, sweet taste coordination, no hygroscopicity, a, azymic high without carious tooth, stability and can not cause the advantages such as digestive discomfort.It can pass through Production by Microorganism Fermentation, yield approximately 50%, and have a wide range of applications in the food industry such as candy, beverage, bakery and appetizing food.Antierythrite is a kind of novel polyalcohols sweetener, extensively be present in Mycophyta (as marine alga, mushroom etc.), fruit (muskmelon, grape etc.) and all kinds of fermented food (as grape wine, chewing gum, pure mellow wine, soy sauce etc., at human or animal's tissue and body fluid, as also there is antierythrite composition in blood, seminal fluid, urine.
Sugar alcohol is the hydrogenating reduction product of a class sugar, is a kind of low-heat, is difficult to digestion, new function type sweetener that sugariness is lower, along with its application in food is increasingly extensive, about the analytical approach of glycitols, also has a lot of research.While adopting HPLC to measure sugar alcohol or sugar, this does not absorb sugar alcohol and sugar in ultraviolet region or visible-range, without fluorescence, adopt differential refraction detector to detect, but differential refraction detector sensitivity is low more yet, and quantitatively level is only 10
-1the g/L order of magnitude.Evaporative light-scattering detector (Evaporative Light ScaltefingDetector, English abbreviation is ELSD) be the detecting device in recent years just appearing in the newspapers, ELSD is not to absorbing the compound of ultraviolet light or fluorescence, as the lipids such as sugar, amino acid, triglyceride detect, there is very high sensitivity, can complement the deficiency of the detecting devices such as ultraviolet or fluorescence.For example, use high performance liquid chromatography-evaporative light-scattering detection method such as Cai Xinxin has been set up the analytical approach of fructose, glucose, sucrose, lactose and maltose in food; The people such as Yu Chen the have studied tablets by HPLC-ELSD content of sugar alcohol in sugar-free cake.Gas chromatography determination carbohydrate, has the advantages such as selectivity is good, amount of samples is few, quick, sensitivity is high, is at home and abroad widely applied in recent years.Adopt gas chromatography determination carbohydrate, the subject matter running into is that carbohydrate itself does not have enough volatility, must first be converted into volatile derivatives and just can measure.For polysaccharide, need be first degraded to monose simple in structure or oligosaccharides, be then derivatized to volatile, heat-staple derivant, by qualitative, quantitative measurement to degraded sugar derivatives, can obtain basic composition and the structure of polysaccharide.The use GC methods such as Adams are analyzed and researched to derivative products such as the organic acid in plant tissue extract, sucrose, glucose, fructose, sweet mellow wine, sorbierites.The chromatography of ions is the most active in recent years, one of liquid chromatography field with fastest developing speed.The principle of sulfate by ion chromatography Saccharide and saccharide alcohols is that carbohydrate, glycitols molecule have galvanochemistry activity and in strong base solution, be ionization state, in the leacheate of high pH value, they can partly or entirely exist with anionic form, can on anion-exchange column, be retained and obtain separation.The main pulsed amperometric detecting device that uses gold electrode of sulfate by ion chromatography sugar, because when applying a current potential on gold electrode, sugar is easily in gold electrode surfaces generation oxidation reaction.Under alkali condition, with gold electrode, detect sugar very sensitive, can detect the sugar of pmol/L, and not need derivatization reaction and complicated Sample Purification on Single to process.In addition, dyestuff intermediate can not, for sugared detection, be mainly because sugared oxidation product produces irreversible pollution to electrode.
For the analysis of sugar alcohol, while adopting vapor-phase chromatography or GC-MS to measure, because the boiling point of sugar alcohol is higher, be difficult to gasification, volatile derivant must be translated into and just GC mensuration can be carried out.While adopting HPLC to measure sugar alcohol, because itself does not absorb at ultraviolet region or visible-range, also without fluorescence, so sugar alcohol adopts differential refraction detector to detect more, but differential refraction detector sensitivity is low, and quantitatively level is only 10
-1the g/L order of magnitude.Method by derivatization is prepared into sample component to have uv absorption and maybe can send the material of fluorescence, and with ultraviolet, diode array or fluorescence detector, sensitivity for analysis can improve greatly, and quantitatively level reaches 10
-2the g/L order of magnitude, but sample preparation trivial operations, and need to select suitable derivatization reagent.The chromatography of ions is compared with existing vapor-phase chromatography, high performance liquid chromatography, capillary electrophoresis etc., have need not derive, easy to operate, highly sensitive and eco-friendly advantage, also fine to the detection accuracy of sugar alcohol and reappearance.
Three, summary of the invention
Concrete research contents of the present invention is mainly divided into following components:
1. determine the pre-treating method that actual sample detects.Sample pre-treatments should be noted that following four aspects: sugar alcohol loss is more few better; Pre-treatment step is more few better; It is more simply better to operate; Consumptive material consuming time is more few better.Pre-treatment generally comprises extraction, removal of impurities, three steps of filtering membrane, then goes up instrumental analysis.Sugar alcohol belongs to water-soluble substances, so adopt intermediate water sample is diluted and extract, ultrasonic is to commonly use the most and simple and effective dissolution extracting mode, the sugar alcohol release that can accelerate in sample is dissolved in aqueous solution, method water-soluble, ultrasonic extraction that this patent adopts, determines ultrasonic extraction time by testing.The material that has residue after water-soluble dilution is also ultrasonic, centrifugal 10min-60min under the rotating speed of use 8000r/min-9000r/min, to remove solid insoluble (material of water-soluble rear clarification can save this step), get the supernatant that is dissolved with sugar alcohol and partly cross through 0.2 μ m-0.3 μ m nylon leaching film and filter, leaving and taking filtrate, to make ion chromatography standby.
2. by screening chromatographic column, explore the impacts of factor on sugar alcohol separating effect such as concentration, flow velocity, column temperature of mobile phase, comprehensive each factor, determines the optimum chromatogram condition of ion chromatography antierythrite.The method of having set up is carried out to methodological study, determine detection limit, determination limit and the range of linearity of each sugar alcohol.
Because sugar alcohol belongs to nutritional substance, the preparation of the direct water of standard items is easy to microbiological contamination, so the compound method adopting should be able to guarantee that each composition to be measured all can obtain accurately qualitatively, on basis, can suitably improving guaranteeing the quality the time of standard items.By consulting pertinent literature, select the sodium azide of 20mg/L to replace water preparation standard items, antierythrite solution is 5.0mg/L.
Sugar alcohol is weak acid, pKa value 12～14.In strong alkali solution, when its pH value is greater than sugared pKa value, the part or all of dissociation of sugar meeting, exists in solution with anionic form, therefore can use NaOH as leacheate, carries out anion exchange separation.Pulsed amperometric detecting device is the detecting device that new development is in recent years got up, select its main advantage to be embodied in its testing conditions consistent with leacheate separation condition, without derivative, its same sugar, sugar alcohol and alcohol compound of requiring exists with the form of hydroxyl negative ion under strong alkaline condition.Due to the oxidizing potential lower (0.1V) of hydroxyl, so matrix disturbs less, can obtain good reappearance and accuracy.
By comparing the anion-exchange column that sugar alcohol is analyzed that can be used for of four kinds of different fillers, screening is applicable to the chromatographic column that antierythrite is analyzed.For mobile phase NaOH, in other conditions fixedly in the situation that, by relatively four kinds of mobile phase concentration 1000mmol/L, 750mmol/L, 500mmol/L and 250mmol/L impacts on the separating effect of sugar alcohol and retention time, select suitable naoh concentration as degree concentration such as grade or gradient concentration elution requirement.In the situation that other conditions are constant, by comparing the different in flow rate such as 0.2ml/min, 0.3ml/min, 0.4ml/min and 0.5ml/min to sugar alcohol and the retention time of sugar and the impact of separating effect, select to be applicable to mobile equality flow velocity or the gradient flow velocity that antierythrite is analyzed.Select different column temperatures: test for 20 ℃, 30 ℃, 35 ℃ and 40 ℃, investigate the impact of column temperature antierythrite retention characteristic.
The present invention has obtained a kind of method for quantitatively determining of antierythrite, and the recovery reaches 85%～90%, have accuracy high, need not derive, easy and simple to handle, highly sensitive, environmental friendliness and high repeatability and other advantages, be a kind of detection method of practicality.
Four, accompanying drawing explanation
The chemical structural formula of Fig. 1 antierythrite.
Five, embodiment
The present invention selects chromatography of ions and anion-exchange column to carry out the stratographic analysis of sugar alcohol, in strong alkali solution when its pH value is greater than the pKa value of sugar alcohol, the part or all of dissociation of sugar alcohol meeting, with anionic form, exist in solution, in view of the pKa value of sugar alcohol is 12～14, therefore use larger concentration hydrogen sodium oxide molybdena as leacheate, carry out anion exchange separation, its concentration is tested and determined.
Chromatographic condition is: NaOH is as mobile phase; 30 ℃ of column temperatures; pulsed amperometric detecting device; flow velocity is 0.4ml/min, and chromatographic column is DIONEX Carbopac PA10 anion analysis post (4mm * 250mm), DIONEX Carbopac PA10 negative ion guard column (4mm * 50mm).Mobile phase concentration a is 1000mmol/L, and concentration b is 750mmol/L, and concentration c is 500mmol/L, and concentration d is 250mmol/L, compares under a, b, c, tetra-kinds of concentration of d the analysis result of antierythrite.
Analyze the result of the mobile phase of relatively above four kinds of variable concentrations, mobile phase concentration is larger, and the retention time of sugar alcohol is shorter, and this effect is along with material retention characteristic grows from weak to strong and obvious gradually, during mobile phase NaOH 500mmol/L, the separating effect of antierythrite is best comparatively speaking.Comprehensive each factor, determines and selects the NaOH of 500mmol/L as mobile phase, adopts Isocratic clution.
Embodiment 2
Tentatively drafting chromatographic condition is: 500mmol/L NaOH is as mobile phase isocratic elution; 30 ℃ of column temperatures; pulsed amperometric detecting device (gold electrode), chromatographic column is DIONEX Carbopac PA10 anion analysis post (4mm * 250mm), DIONEXCarbopac PA10 negative ion guard column (4mm * 50mm).Fixing above condition, the impact of more different flow rate of mobile phase on analysis result, flow velocity a is 0.2ml/min, and flow velocity b is 0.3ml/min, and flow velocity c is 0.4ml/min, and flow velocity d is 0.5ml/min.Because Carbopac PA10 chromatographic column has flow restriction, so consider to compare under a, b, these four kinds of flow velocitys of c, d the ion chromatography result of antierythrite.
When flow rate of mobile phase is 0.2ml/min, the retention time of antierythrite is in 21min left and right; When flow rate of mobile phase is 0.3ml/min, the retention time of antierythrite is in 14min left and right; When flow rate of mobile phase is 0.4ml/min, the retention time of antierythrite is in 11min left and right, and degree of separation is best; When flow rate of mobile phase is 0.5ml/min, the retention time of antierythrite is in 8min left and right; When doing stratographic analysis work, optimal result should be that degree of separation is more good better, and therefore selecting flow rate of mobile phase is 0.4mL/min.
Embodiment 3
Research discovery is in anion-exchange chromatography, and the reservation of sugar alcohol is an exothermic process (raises with temperature, retain and weaken).But every kind of sugar alcohol is subject to the influence degree of temperature different.So, fixing above chromatographic condition, the relatively analysis result of 20 ℃, 30 ℃, 35 ℃, 40 ℃ four kinds of different column temperatures.Compare 20 ℃, 30 ℃, 35 ℃, the 40 ℃ stratographic analysis results that four kinds of different column temperatures are corresponding, visible, along with the reduction of column temperature, retention time increases.Then, also occur a phenomenon, when column temperature is 30 ℃, the chromatographic peak of antierythrite and impurity does not reach baseline separation, and when column temperature is 35 ℃, the chromatographic peak of antierythrite and impurity is completely separated, and therefore, selecting column temperature is 35 ℃.
Embodiment 4
The length of ultrasonic time all discharges more than 95% sugar alcohol in should be able to guaranteeing between sample at this moment.Conventionally, liquid food and semi-solid food products, required ultrasonic time should be shorter than solid food, and gel-based candy is a longest based food consuming time, so selection gel-based candy is model.
First take the gel-based candy of certain mass, with 1000ml intermediate water constant volume, dilute, when ultrasonic 10min, 20min, 30min, 40min, 50min, 60min, get respectively 10ml solution, through 0.22m nylon leaching film, filter, get filtrate for ion chromatography, calculate gel-based candy in the quality of the sugar alcohol of corresponding ultrasonic time stripping.Result demonstration, after ultrasonic 40min, the stripping quantity of antierythrite no longer increases, can think, now all strippings of gel-based candy mesoerythrit.For all the other bread and cheeses, required ultrasonic time is less than this time conventionally.So, select ultrasonic 40min as the ultrasonic extraction time of antierythrite sugar alcohol.
Claims (6)
1. a detection method for antierythrite, is characterized in that adopting water-soluble, ultrasonic processing and with after membrane filtration, with anion-exchange chromatography-pulsed amperometric, quantitatively detects antierythrite.
2. the detection method of a kind of antierythrite as claimed in claim 1, is characterized in that: the ultrasonic ultrasonic processing of the water-soluble rear use of the sample 10-60min that is treated to.
3. the detection method of a kind of antierythrite as claimed in claim 1, is characterized in that: membrane filtration is the solution of getting after the ultrasonic processing of 10ml-15ml, through 0.2 μ m-0.3 μ m nylon leaching film, filters, and gets filtrate for ion chromatography.
4. the detection method of a kind of antierythrite as claimed in claim 1, is characterized in that: the NaOH that the mobile phase of anion-exchange chromatography is 250mmol/L-1000mmol/L is as mobile phase, and flow rate of mobile phase is 0.2mL/min-0.5mL/min.
5. the detection method of a kind of antierythrite as claimed in claim 1; it is characterized in that: the chromatographic column of anion-exchange chromatography is DIONEX Carbopac PA10 anion analysis post (4mm * 250mm), DIONEX Carbopac PA10 negative ion guard column (4mm * 50mm), column temperature is 20 ℃-40 ℃.
6. the detection method of a kind of antierythrite as claimed in claim 1, is characterized in that: detect and be limited to 4.62～100.05 μ g/L, the range of linearity is all across three orders of magnitude, and precision, stability, reappearance test RSD are all less than 5%.
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| CN201210360900.8A CN103675114A (en) | 2012-09-26 | 2012-09-26 | Method for detecting erythritol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105319307A (en) * | 2014-06-12 | 2016-02-10 | 饶君凤 | Analytic method of detecting monosaccharide composition in crocus sativus polysaccharide |
| CN105675758A (en) * | 2016-01-27 | 2016-06-15 | 山东出入境检验检疫局检验检疫技术中心 | Method for simultaneously detecting multiple sugars and sugar alcohols in dairy products |
-
2012
- 2012-09-26 CN CN201210360900.8A patent/CN103675114A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105319307A (en) * | 2014-06-12 | 2016-02-10 | 饶君凤 | Analytic method of detecting monosaccharide composition in crocus sativus polysaccharide |
| CN105675758A (en) * | 2016-01-27 | 2016-06-15 | 山东出入境检验检疫局检验检疫技术中心 | Method for simultaneously detecting multiple sugars and sugar alcohols in dairy products |
| CN105675758B (en) * | 2016-01-27 | 2018-02-09 | 山东出入境检验检疫局检验检疫技术中心 | A kind of while detection is containing the method for a variety of sugar and sugar alcohol in dairy products |
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Application publication date: 20140326 |