CN104568547A - Method for preparing standard carmine sample colorant for analyzing food - Google Patents
Method for preparing standard carmine sample colorant for analyzing food Download PDFInfo
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- CN104568547A CN104568547A CN201510039211.0A CN201510039211A CN104568547A CN 104568547 A CN104568547 A CN 104568547A CN 201510039211 A CN201510039211 A CN 201510039211A CN 104568547 A CN104568547 A CN 104568547A
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Abstract
The invention discloses a method for preparing a standard carmine sample colorant for analyzing food and relates to a synthesis method of the colorant for analyzing the food. The method comprises the following steps that firstly, a mixed solvent composed of aqueous sodium chloride solution and % ethyl alcohol is re-crystallized in four times, a prepared filter cake enters an NF separating membrane device for removal of sodium chloride after being dissolved in water, and the prepared filter cake is concentrated until the conductivity does not decline basically; and the concentrated liquid is dried, crushed and sieved to prepare a standard sample. The carmine colorant is re-crystallized in four times by the mixed solvent composed of 13% aqueous sodium chloride solution and 95% ethyl alcohol. The concentrated liquid is dried and crushed at 90 DEG C and screened by a 60-mesh sieve to prepare the standard sample. The standard value of the national standard synthetic colorant sample is improved in accuracy by scientifically verifying uniformity and steadiness of the synthetic colorant and strictly controlling the impurity content of the raw material, and the uncertainty can be relatively scientifically, reasonably and comprehensively evaluated.
Description
Technical field
The present invention relates to a kind of analysis agent synthetic method, particularly relate to a kind of food analysis carmine red standard sample stainer preparation method.
Background technology
Food analysis synthetic coloring matter national standard sample is the urgent need solving Present Domestic Food Inspection, for government's product quality supervision provides strong technical support.
The purity of current food supervisory detection field to the monitoring Chinese Home standard model of synthetic coloring matter in food is lower, impure relatively high, brings a general difficult problem for interference to testing.
Current China Certified Reference Materials on Food Safety Test, its development level still has many deficiencies:
(1) kind is few, can not satisfy the demand.Although China promulgate the standard model relating to food safety detection oneself about reach kind more than 120, only account for about 6% of standard model sum.Not only quantity is few for the Certified Reference Materials on Food Safety Test of China, and concentration range is narrow, far can not meet the needs of present food security detection technique development.
(2) China's varieties of food items safety detection standard model disparate development.For standard model, wherein 70 numerous food safety detection standard models, pesticide accounts for 12%; Geological and mineral composition class accounts for 7%; Environmental chemical analysis class accounts for 25%; Clinical-chemical analysis and medication components analysis classes account for 50%; Food ingredients analysis classes accounts for 6%.Compared with the current situation of varieties of food items safety detection technology relative equilibrium, the development pole of Certified Reference Materials on Food Safety Test is uneven, and wherein shared by food ingredients analysis classes standard model, the structure proportion of all foods safety detection standard model is obviously on the low side; Food microorganisms class, transgenosis class, animal derived materials class etc. are all then blank.
(3) definite value is main mainly with unit, causes and uses inconvenience.In existing Certified Reference Materials on Food Safety Test, there is sterling, also have matrix examination criteria sample and synthetic coloring matter country.Single composition class standard sample is more, and mostly some standard models particularly succeeded in developing in early days are the element of some macroscopic views of definite value and some elements targetedly, as Pb, Cd, As etc.Like this, when analyzing many components sample, such as, composite pesticide uses the standard model of single component, and one-shot measurement can not obtain analysis result, often needs duplicate measurements, both impact analysis speed, easily again introduces error because of the change of analysis condition.
(4) due to Certified Reference Materials on Food Safety Test own characteristic, and make it develop to be affected.Generally speaking, Certified Reference Materials on Food Safety Test poor stability, moisture-sensitive are mouldy, have very high requirement to preparation, packaging, Techniques of preserving.Except carrying out except irradiation sterilization in preparation process, large multipair storage process proposes the requirement of deepfreeze, and as pork liver requires at-18 DEG C, Pb, Cd in cow's serum composition and whole blood require-20 DEG C etc.
(5) price is high, and impact generally uses.At present, due to Certified Reference Materials on Food Safety Test development and retain costs higher, supplier is few in addition, causes its price also higher, and this have impact on the development of Certified Reference Materials on Food Safety Test largely and generally uses.As: European Union genetically engineered soybean powder examination criteria sample at home selling price be 1100 yuan/gram (minimum packages), also must buy a series (5 contents levels) simultaneously, and can not singly buy.
Develop serial national standard sample, supervisory detection work for synthetic coloring matter in food is provided purity is high, content accurately, homogeneity and all satisfactory national synthetic coloring matter standard model of stability, the level of the food safety detection of national quality inspection system and ability also will get a promotion simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of food analysis carmine red standard sample stainer preparation method, the method is by synthetic coloring matter homogeneity and the Verification of Science of stability and the strict control of raw material impurity content, improve the accuracy of synthetic coloring matter national standard sample standard value, the evaluation of uncertainty also science, rationally, comprehensively more.
The object of the invention is to be achieved through the following technical solutions:
A kind of food analysis carmine red standard sample stainer preparation method, described method comprises following process: the mixed solvent recrystallization first formed with sodium-chloride water solution and % ethanol four times, after gained filter cake is dissolved in water, enter NF separation membrane device and remove sodium chloride, substantially no longer decline to conductivity, then concentrate; Concentrate is dried, pulverizes, is sieved, and obtains standard model.
Described a kind of food analysis carmine red standard sample stainer preparation method, the mixed solvent recrystallization that described carmine colorant forms with 13% sodium-chloride water solution and 95% ethanol four times.
Described a kind of food analysis carmine red standard sample stainer preparation method, described concentrate, in 90 DEG C of oven dry, is pulverized, and crosses 60 mesh sieves, obtains standard model.
Described a kind of food analysis carmine red standard sample stainer preparation method, described standard model HPLC purity 99.73%, dry agent content 99.7%.
Advantage of the present invention and effect are:
1. food analysis synthetic coloring matter of the present invention can ensure its homogeneity and stability.
2. the present invention is by synthetic coloring matter homogeneity and the Verification of Science of stability and the strict control of raw material impurity content, improves the accuracy of synthetic coloring matter national standard sample standard value, the evaluation of uncertainty also science, rationally, comprehensively more.
3. this synthetic coloring matter standard model meets the requirements of GB/T 15000 " standard model work directive/guide " defined completely.
Accompanying drawing explanation
Fig. 1 is the technology of the present invention route schematic diagram;
Fig. 2 is the carmine colorant chromatogram of the present invention;
Fig. 3 is the carmine colorant mass spectrogram of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The purification schemes of synthetic coloring matter standard model is as follows:
Embodiment:
The preparation of carmine red standard sample: the mixed solvent recrystallization that carmine red standard sample forms with 13% sodium-chloride water solution and 95% ethanol four times, after gained filter cake is dissolved in water, enter NF diffusion barrier pilot-plant and remove sodium chloride, substantially no longer decline to conductivity, then concentrate.Concentrate, in 90 DEG C of oven dry, is pulverized, and crosses 60 mesh sieves, obtains standard model (HPLC purity 99.73%, dry agent content 99.7%).
Sample definite value is analyzed and dirt content test:
(1) select respectively tri-chlorination too titrimetry the purity of synthetic coloring matter is measured to famille rose; Apply the content of high effective liquid chromatography for measuring synthetic coloring matter standard model in addition.
Note: dry agent content system is obtained through mathematical computations by content in kind and loss on drying data.
(2) famille rose carried out film process;
Impurity purifying adopts UF membrane to be that film has selective penetrated property.Membrane separation process be with natural can the macromolecule membrane of Prof. Du Yucang, with outside energy or chemical potential difference for expulsive force, bi-component or multi-component solute are separated with solvent, classification, purification and enrichment method, can be used for liquid and gas.For liquid phase separation, can be used for water solution system, non-aqueous solution system, hydrosol system and the water solution system containing other particulates.
Equipment, instrument: 5L tetra-neck round-bottomed flask; S312 digital display constant speed stirrer; Water Tank with Temp.-controlled PHS-2C type precision acidity meter; DDS-11A type electric conductivity instrument; HP 1100 high performance liquid chromatograph; NF diffusion barrier; Constant Temp. Oven (stainless steel inner container); 10 liters of rustless steel container buckets; Stainless steel drip pan; Nine positive family-use grinders; HPLC analytical test condition; HPLC INSTRUMENT MODEL: HP 1100; Chromatographic column: SUPERCO Discovery; Column temperature: 40 DEG C; Mobile phase: a. ammonium acetate solution: 2g/L; B. methyl alcohol; Concentration gradient: with the corresponding adjustment of each product; Flowing velocity: 1mL/min; Determined wavelength: 428/482/500/508/520/525/527/613/630 nm; UF membrane operating conditions: pressure 2.5MPa, temperature < 35 DEG C; Film average flux 20kg/ ㎡
Synthetic coloring matter after repeatedly recrystallization, after part need adopt the mode of NF membrane to purify further by purification afterwards sample drying, pulverize, be screened into high-purity finished product.The selection of recrystallization solvent, anhydrous ethanol solvent purification effect is better, and not only relative content is higher, and the recovery is also higher.The impact of solvent strength, concentration be 2% sodium-chloride water solution and the mixed solvent purification effect that forms of 95% ethanol the most obvious, and the recovery is also high.The impact of recrystallization number of times, by colorant 2% sodium-chloride water solution and 95% ethyl alcohol recrystallization twice, content brings up to 99.5%, and after recrystallization, purity, then without significantly improving, though increase recrystallization number of times, can not reduce the content of impurity further for the third time.
Orthogonal experiments and analysis, analyze and show that the factor affecting toner recrystallization effect is followed successively by: sodium chloride concentration > recrystallization number of times > baking temperature; 3% sodium-chloride water solution and ethanol make solvent, recrystallization twice, and baking temperature is 80 DEG C.Do demonstration test according under this condition, colorant purity after recrystallization purifying can reach 99.87%, meets the preparation needs of standard model.
The raw material that food analysis synthetic coloring matter national standard sample is selected is high purity reagent, analyze the impurity that may exist in often kind of raw material and to the accurate definite value of impurity content, to guarantee that selected raw material meets the manufacture claim of food analysis synthetic coloring matter national standard sample.Accurate Determining is carried out to the impurity in raw material.
Seen by upper table, in raw material, the content of impurity is all less than 4.5%, and namely main content is all greater than 95.5%.
Colorant uniformity testing
15 bottles are respectively randomly drawed from food analysis synthetic coloring matter national standard sample, corresponding analytical approach is adopted to carry out in bottle food analysis synthetic coloring matter national standard sample and uniformity testing between bottle, measure 15 bottles of representative samples that often kind of food analysis synthetic coloring matter national standard sample is randomly drawed, every bottle is repeated 3 times.
all inspection is analyzed and under identical laboratory condition, is carried out independent mensuration by same operating personnel to the main composition of sample.
Method of analysis of variance is adopted to make uniformity testing mode to measurement result as follows:
For the homogeneity of check sample, if randomly drawed m sample, adopt the experimental technique that precision is high, obtain m group equal precision measurement data under the same conditions as follows:
mean value
mean value
………………………………………………
mean value
If
Sum of squares between groups
Quadratic sum in group
The amount of taking statistics F:
Can know thus, to be degree of freedom be this statistic (
,
) F distribution variable.
According to degree of freedom (
,
) and given level of significance α, the F that check in critical value can be shown by F
αvalue.If the F value calculated by formula is: F<F
α, then think and organize there was no significant difference between interior and group, sample is uniform; If F>=F
α, then have systematic error between each group, namely there are differences between sample.Through inspection F<F
α, there was no significant difference in confirmation group and between group, having good uniformity of food analysis synthetic coloring matter national standard sample.
Colorant stability test:
Choose and divide the food analysis synthetic coloring matter installed national standard sample, preserve on request, adopt corresponding detection method according to first close rear thin principle, measure its mass concentration 6 times.Experimental result shows, the food analysis purity of synthetic coloring matter national standard sample fluctuates in the range of uncertainty of expection standard value.Food analysis is good at 18 months internal stabilities with synthetic coloring matter national standard sample, therefore the term of validity is decided to be 18 months (the food analysis synthetic coloring matter national standard sample term of validity calculates from the research and production of metallurgical standard sample date).
The stability test of food analysis synthetic coloring matter national standard sample adopts SPSS 15.0 statistical analysis software to carry out data processing, and detailed results sees appendix 2.
According to GB/T15000 " standard model work directive/guide " regulation, degree of freedom is n-2 and p=0.95(95% confidence level) the student distribution t factor equal 2.78.The t value of synthetic coloring matter and s (b
1) as follows:
The analysis of colorant definite value and standard value are determined:
Through homogeneity and the qualified standard model of stability test, in definite value is analyzed, observe following rule:
(1), by analyzing the analytical approach adopted gather, and calculate the arithmetic mean of these group data.
(2), adopt Xia Piluo-Weir gram (SHAPIRO-WILK) method to carry out test of normality to above-mentioned average data, work as W>W
(α .n )then Normal distribution test is qualified.
(3), when 8 cell mean data fit normal distribution, test of outlier is carried out by Rod Dixon (Dixon) method, when minimum value and maximal value are all less than D
(α .n )during critical value, be then up to the standards, show that being as good as constant value exists.Detailed data sees appendix 4:
(4), calculate its total arithmetic mean and standard deviation, standard deviation numerical digit adopts only enters the method revision of the convention do not given up, and the numerical digit of standard value is alignd with standard deviation numerical digit, carries out the revision of the convention to super digit data by GB/T8170 " numerical value rule for rounding off ".
By GB/T15000 " standard model work directive/guide " regulation, determine the standard value of food synthetic coloring matter chemical analysis national standard sample, program is as follows:
Gather by analyzing the analytical approach adopted, and calculate arithmetic mean and the standard deviation of these group data, standard deviation numerical digit adopts only enters the method revision of the convention do not given up, the numerical digit of standard value is alignd with standard deviation numerical digit, carries out the revision of the convention to super digit data by GB/T8170 " numerical value rule for rounding off ".
The uncertainty evaluation of colorant national standard sample:
The food analysis standard deviation of the uncertainty measured value of synthetic coloring matter national standard sample fixed value determining replaces, the standard deviation of measured value.
。colorant sample homogeneity uncertainty:
By method of analysis of variance inspection food analysis synthetic coloring matter national standard sample homogeneity, data see appendix 1.
According to GB/T 15000.3-2008 " standard model work directive/guide " requirement, uncertainty S2bb=(the MSamong-MSwith)/n of standard model homogeneity.
Colorant stability uncertainty:
The mass concentration change of often kind of food analysis synthetic coloring matter national standard sample is very little, and the stability of sample is good in segment limit when measuring.
The uncertain angle value introduced by stability can according to GB/T 15000.3-2008 " standard model work directive/guide " requirement, the uncertainty U of standard model long-time stability
lts=S
b* t.Wherein S
bthe results are shown in Table effectively 18 months often that 6, t is STABILITY MONITORING.
Colorant uncertainty is become to be synthesized by three parts: the uncertainty of the uncertainty that the analysis of standard model definite value is introduced, the uncertainty of Composite Seismogram homogeneity introducing, stability introducing;
In sum, being introduced not by standard model definite value of food analysis synthetic coloring matter national standard sample
The uncertainty that degree of certainty, homogeneity are introduced and uncertainty three part that stability is introduced are synthesized into.
Carmine colorant uniformity testing data are as follows:
Carmine colorant stability data is as follows:
ANOVA(b)
A Predictors:(Constant), the time
B Dependent Variable: carmine
Coefficients(a)
A Dependent Variable: carmine.
Claims (4)
1. a food analysis carmine red standard sample stainer preparation method, it is characterized in that, described method comprises following process: the mixed solvent recrystallization first formed with sodium-chloride water solution and % ethanol four times, after gained filter cake is dissolved in water, enter NF separation membrane device and remove sodium chloride, substantially no longer decline to conductivity, then concentrate; Concentrate is dried, pulverizes, is sieved, and obtains standard model.
2. a kind of food analysis carmine red standard sample stainer preparation method according to claim 1, is characterized in that, the mixed solvent recrystallization that described carmine colorant forms with 13% sodium-chloride water solution and 95% ethanol four times.
3. a kind of food analysis carmine red standard sample stainer preparation method according to claim 1, is characterized in that, described concentrate, in 90 DEG C of oven dry, is pulverized, and crosses 60 mesh sieves, obtains standard model.
4. a kind of food analysis carmine red standard sample stainer preparation method according to claim 1, is characterized in that, described standard model HPLC purity 99.73%, dry agent content 99.7%.
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Application publication date: 20150429 |