CN103091451B - Detection method of glycerol monostearate alpha crystal - Google Patents
Detection method of glycerol monostearate alpha crystal Download PDFInfo
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Abstract
The invention provides a detection method of glycerol monostearate alpha crystal and belongs to the technical field of analysis. According to the detection method, a measurement method based on a periodate oxidation method is adopted on the basis of a glycerol monostearate alpha crystal method, and critical control points in the detection process are limited to determine an optimal treatment manner of sample pretreatment and the optimal time for titrating sodium thiosulfate. Precision and accuracy experiments of the method show that the method reproducibility and sample recovery rate of the method are much higher than a method I and a method II in the prior art, and the detection method can meet the needs of quantitative detection on the glycerol monostearate alpha crystal in industry.
Description
Technical field
The invention belongs to analysis technical field, be specifically related to a kind of detection method of single stearic acid glycerine lipoprotein alpha-crystal.
Background technology
Emulsifying agent is the surfactant that a class has hydrophilic group and hydrophobic group.Its hydrophilic group is generally the water-soluble group that maybe can be readily wetted by water, as hydroxyl; Its lipophilic group is generally the hydrocarbon long key similar to alkane in lipid structures, therefore can dissolve each other with grease, as modal single stearic acid glycerine lipoprotein, there is the hydroxyl that two hydrophilic, the octadecyl of an oleophylic, therefore oil and two kinds, water can be adsorbed on respectively mutually on the practising physiognomy of repulsion, form thin molecular layer, reduce the interfacial tension of two-phase, thus make original mutual exclusive material be able to Homogeneous phase mixing, form the dispersed system of homogeneous state, change original physical state, and then improve the inner structure of food, improve quality.
Mono fatty acid glyceride (is called for short monoglyceride, MG) be a kind of very important non-ionics, it has good emulsibility, dispersiveness, lubrication and solubilising, is thus widely used in the industry such as food, medicine, cosmetics, printing and dyeing, intermetallic composite coating.In the industrial production, monoglyceride is grease glyceryl alcohol solution and fatty acid and glycerine direct esterification mainly, and in product, the content of monoglyceride is generally 40%-55%.At present, the report about α-monoglyceride content assaying method is a lot, but these method minutes are longer, and complex operation, easily brings error to measurement result, and therefore α-content of monoglyceride assay method still needs to further investigate.
Current α-content of monoglyceride assay method many employings periodate oxidation method determination method, the principle that periodate oxidation method measures α-monoglyceride is: by periodic acid acetum oxidation vicinal hydroxyl groups, then also measure excessive periodic acid with sodium thiosulfate volumetric solution with d8.α-monoglyceride often consumes a part periodic acid, and the iodine that dissociates just reduces a part, the sodium thiosulfate consumed corresponding minimizing two molecule, with the periodic acid solutions as controls liquid of equivalent, the difference of the sodium thiosulfate equivalents that titration reference liquid and sample solution consume, is the equivalents of α-MG
Summary of the invention
Hair adhesion, Ni Yongquan in " research of α-monoglyceride content assaying method " literary composition relatively following two kinds of methods in the strengths and weaknesses of mensuration α-monoglyceride.Author thinks that method two is simple to operate, consuming time few, has more advantage compared to method one.
Method one: dissolve with chloroform after taking suitable amount *; 50mL is diluted to chloroform; Each 25mL aqueous citric acid solution washs 3 times; Measure 50mL periodic acid and 50mL sample chloroform mixes, leave standstill 30min, carry out blank test under the same conditions; Add the liquor kalii iodide of 20ml15%, place after being greater than 30min and add 100mL water, use sodium thiosulfate solution titrated.
Method two: dissolve with chloroform after taking suitable amount *; 100mL is diluted to chloroform, and constant volume; With the mixing of 100mL5% acetic acid solution, leave standstill 1-3h; Measure 50mL periodic acid and 50mL sample chloroform mixes, leave standstill 30min, carry out blank test under the same conditions; Add the liquor kalii iodide of 20ml15%, add 100mL water after placing 1-5min, use sodium thiosulfate solution titrated.
Inventor is on the basis of these two kinds of assay methods of further investigation, and think that although method two has some superiority relative to method one according in a large amount of experimental datas and theoretical basis, but its sample removal of impurities before sample and periodic acid react is thorough, can have an impact to final measurement result; Method one complicated operation, consuming time longer, and in washing process, cause the loss of sample.And person's two kinds of methods are not elaborated to some emphasis indexs, cause operability poor, measurement result and real content produce deviation.For above-mentioned technological deficiency, inventor is on the basis of the detection method of above-mentioned two kinds of single stearic acid glycerine lipoproteins, a kind of method of mensuration single stearic acid glycerine lipoprotein content is newly proposed, the method is simple to operate, consuming time shorter, and the accuracy of method and favorable reproducibility, the content detection of very suitable single stearic acid glycerine lipoprotein uses.
The detection method of single stearic acid glycerine lipoprotein of the present invention, it comprises the steps:
1) sample preparation: get appropriate amount of sample chloroform and dissolve, uses chloroform to be settled to 100mL, can obtain sample solution after filtering;
2) sample removal of impurities: add 300mL10% formic acid-aqueous solution and stir concussion under the environment temperature of 5-15 DEG C in sample solution, after static layering 1-3h, bottom is the sample chloroformic solution after removal of impurities;
3) periodic acid reaction: the sample chloroformic solution measured after 50mL periodic acid and 50mL removal of impurities mixes, after leaving standstill 30min, add the liquor kalii iodide of 20ml15%, 100ml water is added after reaction 10-15min, use the titration of 1mol/L sodium thiosulfate, the volume consuming the sodium thiosulfate of 1mol/L is V1;
4) blank: measure 50mL periodic acid with through step 2) wash after 50mL chloroformic solution mix, after leaving standstill 30min, add the liquor kalii iodide of 20ml15%, 100ml water is added after reaction 10-15min, use the titration of 1mol/L sodium thiosulfate, the volume consuming the sodium thiosulfate of 1mol/L is V2;
5) α-monoglyceride calculates: in sample, the amount of substance of α-monoglyceride is (V2-V1) × 1mol/L.
Although single stearic acid glycerine lipoprotein is water insoluble, but itself and hot water strongly shake when mixing and dispersible in the hot water, in the detection method of the alpha-crystal of single stearic acid glycerine lipoprotein therefore described above, should carry out in low temperature environment in sample dedoping step as far as possible, the present invention carries out under being preferably the environment temperature environment of 5-15 DEG C, is more preferably in the cold water of 10 DEG C and carries out.
In the detection method of the alpha-crystal of single stearic acid glycerine lipoprotein described above, be mainly removing polar impurity and other impurity in sample dedoping step, therefore should add the stronger solvent of polarity, the present invention is preferably the aqueous formic acid of 10%.The polarity of formic acid is greater than acetic acid, and the volume increasing polar solvent can strengthen the impurity-eliminating effect of sample further.Should stir concussion immediately after sample solution mixes with aqueous formic acid, wherein the stirring concussion time is no less than 2min.
In the detection method of the alpha-crystal of single stearic acid glycerine lipoprotein described above, the time that sodium thiosulfate starts titration is the important reference mark affecting laboratory test results.Titration is too early, and reaction not yet completes, and the sharp increase of liquor capacity makes reaction slow down, and causes the volume consuming sodium thiosulfate less than normal; React long, then the iodine in solution may volatilize, and causes the volume consuming sodium thiosulfate less than normal.Inventor confirms by experiment, and when periodic acid and potassium iodide react 10-16min, react the preferred titration time substantially completed as sodium thiosulfate, further preferably, the preferred titration time of sodium thiosulfate is 12-14min.
The determination of experimental example sodium thiosulfate titration time
Measuring sodium thiosulfate titration time in detection method according to the alpha-crystal of single stearic acid glycerine lipoprotein of the present invention, take solution turned blue as titration end-point.Its measurement result is as shown in table 1.
The volume of sodium thiosulfate is consumed during table 1 differential responses time titration
As can be seen from Table 1, the consumption volume of sodium thiosulfate rises gradually in reaction 2min-10min, remains constant, decline gradually after 18min in 10min-16min.React completely when this shows between 10min-16min, and the content constant of the iodine generated, should be the Best Times of sodium thiosulfate titration.
The detection method of single stearic acid glycerine lipoprotein alpha-crystal of the present invention has following advantage relative to prior art:
1) detection method preci-sion and accuracy experiment display, the method reappearance of detection method and average recovery, far above method one of the prior art and method two, can meet in industry the needs that single stearic acid glycerine lipoprotein alpha-crystal quantitatively detects.
2) detection method determines the optimum polarity solution in sample removal of impurities stage, and its impurity-eliminating effect improves the purity of material to be checked in sample chloroformic solution relative to prior art, ensure that the accuracy of detection method.
3) detection method is determined through experimentation the best titration time of sodium thiosulfate, its volatilization having considered reacting finisheding degree and generated material, further increases the precision of detection method.
Embodiment
Further describe the present invention below by way of specific embodiment, the present invention is not limited only to following examples.Within the scope of the invention or not departing from content of the present invention, spirit and scope, the change carried out the present invention, combination or replacement, be apparent for a person skilled in the art, and be included within the scope of the present invention.
Embodiment 1 detection method compares with the preci-sion and accuracy of method one and method two
1, preci-sion and accuracy of the present invention measures
1.1 precision test
1.1.1, collimation test
Get the same sample 6 parts containing single stearic acid glycerine lipoprotein, carry out 6 collimation experiments by detection method of the present invention simultaneously, calculate its test result as shown in table 2.
Table 2 collimation measurement result (n=3)
1.1.2, method reappearance experiment
Get the same sample containing single stearic acid glycerine lipoprotein, carry out 6 experiments respectively, measurement result is as shown in table 3
Table 3 detection method reappearance measuring result
Precision mainly reflects the size of the stochastic error that analytical approach exists, and measures from collimation and reappearance two character.Wherein collimation Main Analysis surrounding environment error that test method is caused, the error caused by reappearance Main Analysis test apparatus system.From Precision test result, RSD value, about 1.0, illustrates that the precision of detection method is higher.
1.2, accuracy experiment
Table 4 detection method application of sample recovery experiment measurement result
Accuracy is the overall target that detection method exists systematic error and stochastic error, and determines the reliability of analysis result.Reclaim measurement result from table 4 application of sample, average recovery rate is 99.8%, RSD value is 1.61%.From accuracy test result, in this test processing procedure, the loss of sample is less, and accuracy is good.
The preci-sion and accuracy of 2 methods one measures
2.1 method reappearance experiments
Experimental technique is tested with the method reappearance of detection method.
Table 5 method one detection method reappearance measuring result
2.2 application of sample recovery experiments
Experimental technique is with the application of sample recovery experiment of detection method.
Table 6 method one detection method application of sample recovery experiment
3, the preci-sion and accuracy of method two measures
3.1 method reappearance experiments
Experimental technique is tested with the method reappearance of detection method.
Table 7 method two detection method reappearance measuring result
3.2 application of sample recovery experiments
Experimental technique is with the application of sample recovery experiment of detection method.
Table 8 method two detection method application of sample recovery experiment measurement result
Consolidated statement 2-table 9 adopts distinct methods working sample result to show: method one detection method is compared with detection method, measurement result is less than normal, supposition may be because detection method pretreatment process is complicated, the loss of detection material has been there is in sample handling processes, and the stability of method is not strong, and the reappearance of method and recovery experiment are all undesirable.Method two detection method owing to can not determine in the titration time of sodium thiosulfate, and cause its measurement result to same sample to differ comparatively large, the reappearance of method and recovery experiment are also undesirable.The reappearance experiment of the detection method of α-monoglyceride of the present invention and the RSD value of application of sample recovery experiment all lower, industrial α-monoglyceride detection needs can be met.
Claims (2)
1. a detection method for single stearic acid glycerine lipoprotein alpha-crystal, it comprises the steps:
1) sample preparation: get appropriate amount of sample chloroform and dissolve, uses chloroform to be settled to 100mL, can obtain sample solution after filtering;
2) sample removal of impurities: add 300mL10% formic acid-aqueous solution and stir concussion under the environment temperature of 5-15 DEG C in sample solution, after static layering 1-3h, bottom is the sample chloroformic solution after removal of impurities;
3) periodic acid reaction: the sample chloroformic solution measured after 50mL periodic acid and 50mL removal of impurities mixes, after leaving standstill 30min, add the liquor kalii iodide of 20mL15%, 100mL water is added after reaction 10-15min, use the titration of 1mol/L sodium thiosulfate, the volume consuming the sodium thiosulfate of 1mol/L is V1;
4) blank: measure 50mL periodic acid with through step 2) wash after 50mL chloroformic solution mix, after leaving standstill 30min, add the liquor kalii iodide of 20mL15%, 100mL water is added after reaction 10-16min, use the titration of 1mol/L sodium thiosulfate, the volume consuming the sodium thiosulfate of 1mol/L is V2;
5) α-monoglyceride calculates: in sample, the amount of substance of α-monoglyceride is (V2-V1) × 1mol/L.
2. the detection method as described in claim 1, is characterized in that described step 2) environment temperature is 10 DEG C in sample removal of impurities.
3. the detection method as described in claim 1, is characterized in that described step 2) in stir the concussion time be no less than 2min.
4. the detection method as described in claim 1, is characterized in that the reaction time after adding liquor kalii iodide in described step 4) is 12-14min.
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Citations (1)
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| CN1869664A (en) * | 2005-05-25 | 2006-11-29 | 中国石油天然气股份有限公司 | Method for testing purity of recovered ethylene glycol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1869664A (en) * | 2005-05-25 | 2006-11-29 | 中国石油天然气股份有限公司 | Method for testing purity of recovered ethylene glycol |
Non-Patent Citations (3)
| Title |
|---|
| α-单甘酯含量测定方法的研究;毛连生 等;《西部粮油科技》;20010228;第26卷(第1期);第43-44页 * |
| 甘油单硬脂酸酯;罗明生 等;《中国药用辅料》;化学工业出版社;20060430;全文 * |
| 高碘酸氧化法测定油脂中1-单甘酯的含量;栾霞 等;《中国油脂》;20080920;第33卷(第9期);第73-75页 * |
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