CN105466981A - Method for identifying lactogenesis adulteration based on nonlinear chemical fingerprint chromatography technique - Google Patents
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Abstract
The invention relates to a method for identifying lactogenesis adulteration based on a nonlinear chemical fingerprint chromatography technique. The method comprises the following steps: establishing a lactogenesis nonlinear chemical fingerprint chromatography standard database; in the process of detecting the lactogenesis adulteration, comparing the visible shape differences of a to-be-detected lactogenesis sample and a standard lactogenesis nonlinear chemical fingerprint chromatography, calculating the maximal relative standard deviation of the parameter information, calculating the whole similarity, and expressing an identifying result. According to the method provided by the invention, the complex pretreatment, such as, separation, extraction, and the like, is not required, the equipment cost is low, the onsite quick detection can be performed and the detection limit is low; the nonlinear chemical fingerprint chromatography is a cluster representation of all the active ingredients of the sample and has the characteristics of broad spectrum detection; the detection for various doping indexes one by one is not required; the detection cost is low; the method also can be used for detecting the lactogenesis doping with unknown raw material component and judging the doping of the mass of the raw material lactogenesis.
Description
Technical field
The invention belongs to technical field of food safety, particularly relate to the adulterated mirror method for distinguishing of a kind of lactogenesis based on nonlinear chemical fingerprint.
Background technology
Milk and milk products is high nutritive value food indispensable during people live, and milk is the exclusive source of infant in early days except breast milk, and its relationship between quality is to the life security of child.But in recent years, some events caused because of quality of milk powder problem emerge in an endless stream, as " melamine milk powder case ", " the hormone door " of holy unit, " malicious milk powder " event of Fuyang, and nearest " leather milk " etc.These events major reason is caused to be exactly that the quality control of lactogenesis does not pass a test.
In order to obtain more interests, often water is impregnated in lactogenesis, and in order to make the lactogenesis of water mixing reach acquisition criteria, the nonelectrolytes such as neutral salt and urea, sucrose, ox urine such as salt, native salt, saltcake, lead sulfate, chemical fertilizer (sulfate of ammoniac, carbonic acid ammonia), nitrate and nitrite usually need be mixed to improve the proportion of milk; Mix colloidal material to increase the viscosity of milk, there is no thin sense during inspection matter, the various dopant that can increase proportion can be covered again simultaneously; Mix washing powder etc. to increase milk matter turbidity; Mix the alkaloids such as sodium bicarbonate, sodium carbonate, lime water to cover the denaturalization phenomenon that becomes sour; Mix the materials such as amine salt, protein hydrolysate powder, volatile nitrogen to improve nitrogen content; Mixing the preservative substance such as formaldehyde, hydrogen peroxide prevents putrid and deteriorated to reduce microorganism level.Therefore, lactogenesis is adulterated to be generally several or multiple adulterated material and to blend and form, and make its physical behavior, quality index, close to normal lactogenesis, reaches the object of mixing the spurious with the genuine.
The inspection of lactogenesis is the key subjects that country pays much attention to always, and relevant functional department of country also carries out specification, perfect to the definition of lactogenesis and quality standard always.Just promulgate as far back as 1986 " Fresh Milk acquisition criteria (GB/T6914-86) ", within 2010, formulated " lactogenesis hygienic standard (GB19301-2010) ".Establishing criteria, is mainly divided into organoleptic indicator, physical and chemical index and microbiological indicator three major types to the quality requirements of the fresh milk of purchase; Physical and chemical index mainly comprises the projects such as freezing point, relative density, protein, fat, impurity degree, non-fat solid, acidity, heavy metal and the residual beast of agriculture be residual; The method of inspection is the technical method such as Kjeldahl's method, surname extraction, acid base titration, ultimate analysis, stratographic analysis mainly; The defect of protein is surveyed for making up Kjeldahl's method, standard that country puts into effect the mensuration (GB/T21704-2008) of non-protein nitrogen content in dairy products " breast with ", for melamine event, within 2008, also put into effect especially " lactogenesis and melamine in dairy products detection method (GB/T22388-2008) ".
About the discriminating detection method of the adulterated material of lactogenesis, there are many bibliographical informations both at home and abroad.Mainly containing development process (as starch based, urea, hydrogen peroxide etc.), the precipitation method (as saltcake), quick detection test paper method (microbiotic, melamine), physical index (as freezing point, relative density, refraction index etc.) etc. can at the on-the-spot experimental technique carried out of lactogenesis purchase, go back some method can only carried out in laboratory because needing complicated pre-service in addition, as capillary electrophoresis (mastitis), chromatography (melamine), PCR (microbiotic, microorganism), culture of microorganism (microbiotic) etc.Analyze these detection methods can notice: (1) traditional detection method is all carry out screening for the characteristic attribute of a certain known dopants, but to detect one by one all known adulterants, the large cost of workload is high, and helpless especially for the adulterant of the unknown, thus cannot realize the complete detection to raw material milk; (2) some method need to carry out before measuring to be separated, the pre-service such as extraction, cause complex operation, the running time be long, reagent consumption is large, expensive equipment, analysis cost be high, be not suitable for the adulterated diagnostic test that lactogenesis purchase is on-the-spot; (3) for emerging in an endless stream, adulterated technology of all shapes and colors, corresponding detection technique upgrades too slow, and classical " Kjeldahl's method " allows " melamine event " to be called the example allowing people imprint on the bones and the memory; (4) the lactogenesis information categorization that shows of these all technical methods is numerous and diverse, cannot carry out a comprehensive expression.Comprehensive above current deficiency, in the urgent need to providing a kind of without the need to pre-treatment, simple to operate, with low cost and can differentiate various adulterated material (comprise known with the unknown) fast, can identify the technical method of various adulterated means.
Summary of the invention
The object of the invention is for the adulterated means of lactogenesis and current discriminating detection method delayed, lactogenesis examination cannot be met accurately comprehensively technical support is provided, the adulterated method for quick identification of lactogenesis of a kind of energy general token Raw Milk Quality and applicable purchase field test is provided, thus solves Problems existing in background technology.
Technical matters solved by the invention realizes by the following technical solutions:
The adulterated mirror method for distinguishing of lactogenesis based on nonlinear chemical fingerprint, comprises the steps:
(1) lactogenesis nonlinear chemical fingerprint standard database is set up:
A. instrument preheating and correction: open computer, nonlinear chemical fingerprint intelligent analytical instrument main frame, arranging temperature of reactor is 45-55.0 DEG C, magnetic stirring apparatus rotating speed is 1000-1500r/min, add sulfuric acid solution in the reactor, build reactor cap, insert mercurous chloride electrode and platinum electrode, open data acquisition system data to current potential E not t change in time;
B. nonlinear chemical fingerprint detection method: adopt chemical oscillation system, add lactogenesis sample in the reactor, 25mL sulfuric acid solution, 10mL acetone soln and 15mL manganese sulfate solution are in the reactor of band stirrer, the reactor cap building band injection orifice and electrode is placed on nonlinear chemical fingerprint intelligent analytical instrument, adopt 45-55.0 DEG C of water-bath, 1000-1500r/min magnetic agitation, constant temperature also starts timing, when constant speed stirs 5min, inject the sodium bromate solution of 5mL, at once menu image data is clicked, record E-t curve is to current potential E t change no longer in time,
C. the foundation of lactogenesis nonlinear chemical fingerprint and standardization: by the different dairy bread of method establishment described in step (1) b, milk seedbed and the lactogenesis nonlinear chemical fingerprint in galactopoiesis season, and carry out standardization such as data isometric grade, utilize nonlinear chemical fingerprint data handling system, extract the parameter informations such as induction time, oscillation period, the number of oscillation, vibration life-span, rounded breasts time, peak swing, set up the lactogenesis nonlinear chemical fingerprint storehouse of different cultivars, the lactogenesis standard database comparison detected as lactogenesis doping is used;
(2) the adulterated doping lactogenesis of identification is detected:
A. data processing:
I. step (1) gained is detected data importing nonlinear chemical fingerprint data handling system, and be placed in same coordinate with lactogenesis standard finger-print and draw its E-t curve, observe the difference of its shape directly perceived;
Ii. extract the parameter informations such as its induction time, oscillation period, vibration life-span, the number of oscillation, rounded breasts time, peak swing, and compare with lactogenesis standard finger-print parameter information, calculate its relative standard deviation, get maximal value;
Iii. the overall similarity of sample dairy products and standard lactogenesis finger-print is calculated;
B. results expression: be made up of shape matching directly perceived, the maximum relative standard deviation of parameter information and overall similarity, tested lactogenesis sample is divided into qualified, suspicious, defective lactogenesis three conclusions, qualified and defective raw material lactogenesis is classified and is processed, and suspicious lactogenesis sample transfers to other exact instrument to carry out subsequent authentication detection.
Described mercurous chloride electrode and platinum electrode are 217-1 type saturated calomel electrode and 213 type platinum electrodes.
Described sodium bromate solution is injected fast by syringe or liquid-transfering gun.
The concentration that the concentration of described sulfuric acid solution is 1.00mol/L, the concentration of described acetone soln is 10% (V/V) and described manganese sulfate solution be 0.10mol/L, the concentration of described sodium bromate solution be 0.8mol/L.
Described chemical oscillation system is " H
++ Mn
2++ acetone+BO
3 -" system.
The present invention has following beneficial effect:
The present invention is the raw material lactogenesis doping method for quick based on the nonlinear chemical reaction basis under far from equilibrium condition, relative to the method that the doping of traditional lactogenesis detects, this law is without the need to the complicated pre-treatment such as separation and Extraction, and equipment price is cheap, can field quick detection and detection limit is low; Nonlinear chemical fingerprint is the sign of trooping of all active components of sample, and have the advantages that wide spectrum detects, without the need to detecting one by one each doping index, testing cost is cheap; Raw material lactogenesis doping for non-principal component also can detect, and carries out doping judgement, for the purchase of lactogenesis provides technical support to the quality of raw material lactogenesis.
Accompanying drawing explanation
Fig. 1 is normal lactogenesis and the nonlinear chemical fingerprint mixing sucrose 2.000g/100mL;
Fig. 2 is normal lactogenesis and the nonlinear chemical fingerprint mixing animal hydrolyzed protein 2.000g/100mL;
Fig. 3 is normal lactogenesis and the nonlinear chemical fingerprint mixing 30% hydrogen peroxide 1mL/100mL;
Fig. 4 is normal lactogenesis and the nonlinear chemical fingerprint mixing NaCl0.1g/100mL;
Fig. 5 is the nonlinear chemical fingerprint of normal lactogenesis and blending milk;
Fig. 6 is the nonlinear chemical fingerprint of normal lactogenesis and lactogenesis check sample.
Embodiment
The technological means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with concrete diagram, setting forth the present invention further.
To mixing sucrose breast, mixing animal hydrolyzed protein breast, adding H
2o
2breast, mix salt breast, multiple alloy modulation breast and fresh lactogenesis number consecutively 1,2,3,4,5,6 detecting respectively.
The disposition of this example sample: add sucrose 2.000g/100mL (additive concentration is 2%), add animal hydrolyzed protein 2.000g/100mL (additive concentration 2%), add 30% hydrogen peroxide solution 1mL/100mL (additive concentration 0.3%), add 0.1gNaCl (additive concentration 0.1%), the lactogenesis aqueous solution of 75% adds appropriate albumen powder, vegetable fat powder, fatty powder, hydrolyzed vegetable protein, glucose also makes it detect the protein reaching lactogenesis national Specification through dairy products analyser, fat, non-fat solid, the required values such as relative density, fresh lactogenesis is control group.
Embodiment 1:
Get numbering 1 to mix sucrose breast sample solution 10mL and set up its nonlinear chemical fingerprint as follows:
A. instrument preheating and correction: open computer, nonlinear chemical fingerprint intelligent analytical instrument main frame, arranging temperature of reactor is 55.0 DEG C, magnetic stirring apparatus rotating speed is 1000r/min, add the sulfuric acid solution of 1mol/L in the reactor, build reactor cap, insert mercurous chloride electrode and platinum electrode, open data acquisition system data to current potential E not t change in time;
B. nonlinear chemical fingerprint detection method: adopt chemical oscillation system, add lactogenesis sample in the reactor, 25mL1mol/L sulfuric acid solution, the acetone soln of 10mL10% (V/V) and 15mL0.1mol/L manganese sulfate solution are in the reactor of band stirrer, the reactor cap building band injection orifice and electrode is placed on nonlinear chemical fingerprint intelligent analytical instrument, adopt 45-55.0 DEG C of water-bath, 1000-1500r/min magnetic agitation, constant temperature also starts timing, when constant speed stirs 5min, the sodium bromate solution of 5mL0.8mol/L is injected fast by syringe, at once menu image data is clicked, record E-t curve is to current potential E t change no longer in time.
Be placed in same horizontal ordinate with lactogenesis standard finger-print respectively again, see Fig. 1.
Embodiment 2:
Get numbering 2 to mix animal hydrolyzed protein breast sample solution 10mL and set up its nonlinear chemical fingerprint as follows:
A. instrument preheating and correction: open computer, nonlinear chemical fingerprint intelligent analytical instrument main frame, arranging temperature of reactor is 45.0 DEG C, magnetic stirring apparatus rotating speed is 1500r/min, add the sulfuric acid solution of 1mol/L in the reactor, build reactor cap, insert mercurous chloride electrode and platinum electrode, open data acquisition system data to current potential E not t change in time;
B. nonlinear chemical fingerprint detection method: adopt chemical oscillation system, add lactogenesis sample in the reactor, 25mL1mol/L sulfuric acid solution, the acetone soln of 10mL10% (V/V) and 15mL0.1mol/L manganese sulfate solution are in the reactor of band stirrer, the reactor cap building band injection orifice and electrode is placed on nonlinear chemical fingerprint intelligent analytical instrument, adopt 45 DEG C of water-baths, 1500r/min magnetic agitation, constant temperature also starts timing, when constant speed stirs 5min, the sodium bromate solution of 5mL0.8mol/L is injected fast by liquid-transfering gun, at once menu image data is clicked, record E-t curve is to current potential E t change no longer in time.
Be placed in same horizontal ordinate with lactogenesis standard finger-print respectively again, see Fig. 2.
Embodiment 3:
Get numbering 3 and add H
2o
2breast sample solution 10mL sets up its nonlinear chemical fingerprint as follows:
A. instrument preheating and correction: open computer, nonlinear chemical fingerprint intelligent analytical instrument main frame, arranging temperature of reactor is 47.0 DEG C, magnetic stirring apparatus rotating speed is 1100r/min, add the sulfuric acid solution of 1mol/L in the reactor, build reactor cap, insert mercurous chloride electrode and platinum electrode, open data acquisition system data to current potential E not t change in time;
B. nonlinear chemical fingerprint detection method: adopt chemical oscillation system, add lactogenesis sample in the reactor, 25mL1mol/L sulfuric acid solution, the acetone soln of 10mL10% (V/V) and 15mL0.1mol/L manganese sulfate solution are in the reactor of band stirrer, the reactor cap building band injection orifice and electrode is placed on nonlinear chemical fingerprint intelligent analytical instrument, adopt 45 water-baths, 1100r/min magnetic agitation, constant temperature also starts timing, when constant speed stirs 5min, the sodium bromate solution of 5mL0.8mol/L is injected fast by syringe, at once menu image data is clicked, record E-t curve is to current potential E t change no longer in time.
Be placed in same horizontal ordinate with lactogenesis standard finger-print respectively again, see Fig. 3.
Embodiment 4:
Get numbering 4 to mix salt breast sample solution 10mL and set up its nonlinear chemical fingerprint as follows:
A. instrument preheating and correction: open computer, nonlinear chemical fingerprint intelligent analytical instrument main frame, arranging temperature of reactor is 49.0 DEG C, magnetic stirring apparatus rotating speed is 1200r/min, add the sulfuric acid solution of 1mol/L in the reactor, build reactor cap, insert mercurous chloride electrode and platinum electrode, open data acquisition system data to current potential E not t change in time;
B. nonlinear chemical fingerprint detection method: adopt chemical oscillation system, add lactogenesis sample in the reactor, 25mL1mol/L sulfuric acid solution, the acetone soln of 10mL10% (V/V) and 15mL0.1mol/L manganese sulfate solution are in the reactor of band stirrer, the reactor cap building band injection orifice and electrode is placed on nonlinear chemical fingerprint intelligent analytical instrument, adopt 49 DEG C of water-baths, 1500r/min magnetic agitation, constant temperature also starts timing, when constant speed stirs 5min, the sodium bromate solution of 5mL0.8mol/L is injected fast by liquid-transfering gun, at once menu image data is clicked, record E-t curve is to current potential E t change no longer in time.
Be placed in same horizontal ordinate with lactogenesis standard finger-print respectively again, see Fig. 4.
Embodiment 5:
Get numbering more than 5 kind of alloy to modulate newborn sample solution 10mL and set up its nonlinear chemical fingerprint as follows:
A. instrument preheating and correction: open computer, nonlinear chemical fingerprint intelligent analytical instrument main frame, arranging temperature of reactor is 51.0 DEG C, magnetic stirring apparatus rotating speed is 1300r/min, add the sulfuric acid solution of 1mol/L in the reactor, build reactor cap, insert mercurous chloride electrode and platinum electrode, open data acquisition system data to current potential E not t change in time;
B. nonlinear chemical fingerprint detection method: adopt chemical oscillation system, add lactogenesis sample in the reactor, 25mL1mol/L sulfuric acid solution, the acetone soln of 10mL10% (V/V) and 15mL0.1mol/L manganese sulfate solution are in the reactor of band stirrer, the reactor cap building band injection orifice and electrode is placed on nonlinear chemical fingerprint intelligent analytical instrument, adopt 51 DEG C of water-baths, 1300r/min magnetic agitation, constant temperature also starts timing, when constant speed stirs 5min, the sodium bromate solution of 5mL0.8mol/L is injected fast by syringe, at once menu image data is clicked, record E-t curve is to current potential E t change no longer in time.
Be placed in same horizontal ordinate with lactogenesis standard finger-print respectively again, see Fig. 5.
Embodiment 6:
Get numbering 6 fresh lactogenesis sample solution 10mL and set up its nonlinear chemical fingerprint as follows:
A. instrument preheating and correction: open computer, nonlinear chemical fingerprint intelligent analytical instrument main frame, arranging temperature of reactor is 53.0 DEG C, magnetic stirring apparatus rotating speed is 1400r/min, add the sulfuric acid solution of 1mol/L in the reactor, build reactor cap, insert mercurous chloride electrode and platinum electrode, open data acquisition system data to current potential E not t change in time;
B. nonlinear chemical fingerprint detection method: adopt chemical oscillation system, add lactogenesis sample in the reactor, 25mL1mol/L sulfuric acid solution, the acetone soln of 10mL10% (V/V) and 15mL0.1mol/L manganese sulfate solution are in the reactor of band stirrer, the reactor cap building band injection orifice and electrode is placed on nonlinear chemical fingerprint intelligent analytical instrument, adopt 53 DEG C of water-baths, 1400r/min magnetic agitation, constant temperature also starts timing, when constant speed stirs 5min, the sodium bromate solution of 5mL0.8mol/L is injected fast by liquid-transfering gun, at once menu image data is clicked, record E-t curve is to current potential E t change no longer in time.
Be placed in same horizontal ordinate with lactogenesis standard finger-print respectively again, see Fig. 6.
As follows embodiment 1-6 the data obtained is processed:
I. will detect data importing nonlinear chemical fingerprint data handling system, and be placed in same coordinate with lactogenesis standard finger-print and draw its E-t curve, observe the difference of its shape directly perceived;
Ii. extract the parameter informations such as its induction time, oscillation period, vibration life-span, the number of oscillation, rounded breasts time, peak swing, and compare with lactogenesis standard finger-print parameter information, calculate its relative standard deviation, get maximal value;
Iii. the overall similarity of sample dairy products and standard lactogenesis finger-print is calculated.
Obtain the parameter information such as finger-print induction time, oscillation period of each sample and calculate the relative standard deviation of itself and standard lactogenesis finger-print parameter information, in the relative standard deviation of table 1 test sample book and standard lactogenesis nonlinear chemical fingerprint parameter information; Calculate its overall similarity, in the overall similarity of table 2 test sample book and standard lactogenesis nonlinear chemical fingerprint; Identification result is in the adulterated doping identification result of table 3 test sample book.
Table 1
Table 2
Table 3
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and instructions just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (5)
1., based on the adulterated mirror method for distinguishing of lactogenesis of nonlinear chemical fingerprint, it is characterized in that: comprise the steps:
(1) lactogenesis nonlinear chemical fingerprint standard database is set up:
A. instrument preheating and correction: open computer, nonlinear chemical fingerprint intelligent analytical instrument main frame, arranging temperature of reactor is 45-55.0 DEG C, magnetic stirring apparatus rotating speed is 1000-1500r/min, add sulfuric acid solution in the reactor, build reactor cap, insert mercurous chloride electrode and platinum electrode, open data acquisition system data to current potential E not t change in time;
B. nonlinear chemical fingerprint detection method: adopt chemical oscillation system, add lactogenesis sample in the reactor, 25mL sulfuric acid solution, 10mL acetone soln and 15mL manganese sulfate solution are in the reactor of band stirrer, the reactor cap building band injection orifice and electrode is placed on nonlinear chemical fingerprint intelligent analytical instrument, adopt 45-55.0 DEG C of water-bath, 1000-1500r/min magnetic agitation, constant temperature also starts timing, when constant speed stirs 5min, inject the sodium bromate solution of 5mL, at once menu image data is clicked, record E-t curve is to current potential E t change no longer in time,
C. the foundation of lactogenesis nonlinear chemical fingerprint and standardization: by the different dairy bread of method establishment described in step (1) b, milk seedbed and the lactogenesis nonlinear chemical fingerprint in galactopoiesis season, and carry out standardization such as data isometric grade, utilize nonlinear chemical fingerprint data handling system, extract the parameter informations such as induction time, oscillation period, the number of oscillation, vibration life-span, rounded breasts time, peak swing, set up the lactogenesis nonlinear chemical fingerprint storehouse of different cultivars, the lactogenesis standard database comparison detected as lactogenesis doping is used;
(2) the adulterated doping lactogenesis of identification is detected:
A. data processing:
I. step (1) gained is detected data importing nonlinear chemical fingerprint data handling system, and be placed in same coordinate with lactogenesis standard finger-print and draw its E-t curve, observe the difference of its shape directly perceived;
Ii. extract the parameter informations such as its induction time, oscillation period, vibration life-span, the number of oscillation, rounded breasts time, peak swing, and compare with lactogenesis standard finger-print parameter information, calculate its relative standard deviation, get maximal value;
Iii. the overall similarity of sample dairy products and standard lactogenesis finger-print is calculated;
B. results expression: be made up of shape matching directly perceived, the maximum relative standard deviation of parameter information and overall similarity, tested lactogenesis sample is divided into qualified, suspicious, defective lactogenesis three conclusions, qualified and defective raw material lactogenesis is classified and is processed, and suspicious lactogenesis sample transfers to other exact instrument to carry out subsequent authentication detection.
2. the adulterated mirror method for distinguishing of a kind of lactogenesis based on nonlinear chemical fingerprint according to claim 1, is characterized in that: described mercurous chloride electrode and platinum electrode are 217-1 type saturated calomel electrode and 213 type platinum electrodes.
3. the adulterated mirror method for distinguishing of a kind of lactogenesis based on nonlinear chemical fingerprint according to claim 1, is characterized in that: described sodium bromate solution is injected fast by syringe or liquid-transfering gun.
4. the adulterated mirror method for distinguishing of a kind of lactogenesis based on nonlinear chemical fingerprint according to claim 1, is characterized in that: the concentration that the concentration of described sulfuric acid solution is 1.00mol/L, the concentration of described acetone soln is 10% (V/V) and described manganese sulfate solution be 0.10mol/L, the concentration of described sodium bromate solution be 0.8mol/L.
5. the adulterated mirror method for distinguishing of a kind of lactogenesis based on nonlinear chemical fingerprint according to claim 1, is characterized in that: described chemical oscillation system is " H
++ Mn
2++ acetone+BO
3 -" system.
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CN110487878A (en) * | 2019-08-16 | 2019-11-22 | 陕西科技大学 | A kind of adulterated determination method of wide spectrum of fresh sheep cream |
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