Quality control sample effervescent tablet for determining pesticide residues and metal elements as well as preparation method and application of quality control sample effervescent tablet

The preparation of effervescent tablets by mixing freeze-dried fruit and vegetable powder and disintegrant is solved, and the matrix effect problems caused by the auxiliary materials in the detection of pesticide residues and metal elements in the prior art are solved, and the accuracy and stability of the detection are achieved. Suitable for detection of pesticide residues and metal elements.

CN119269194APending Publication Date: 2025-01-07SHANGHAI MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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Patent Information

Application Number
CN202411511559.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-28
Publication Date
2025-01-07

AI Technical Summary

Technical Problem

In the prior art, effervescent tablets cannot be suitable for the field of pesticide residues and metal element detection, and the matrix effect caused by auxiliary materials affects the accuracy of the analysis results.

Method used

Quality-controlled effervescent tablets are prepared by mixing lyophilized fruit and vegetable powder with disintegrant, avoiding the addition of exogenous adhesives and lubricants, and controlling the bonding stability using the content and particle size of fructose to form no external interference. quality control effervescent tablets.

Benefits of technology

The accuracy of pesticide residues and metal element detection is achieved, the interference of auxiliary materials is avoided, the stability and storage of quality control samples is improved, and it is convenient for laboratory use.

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Abstract

The invention relates to the field of pesticide residue detection and element analysis, in particular to a quality control sample effervescent tablet for determining pesticide residues and metal elements as well as a preparation method and application of the quality control sample effervescent tablet for determining the pesticide residues and the metal elements, and the quality control sample effervescent tablet for determining the pesticide residues and the metal elements is prepared by mixing and tabletting a standard sample and a disintegrating agent; the labeled sample comprises freeze-dried fruit and vegetable powder and a standard substance which is added into the fruit and vegetable powder and is used for detecting pesticides and metal elements. The tablet is convenient to use in a laboratory while ensuring the stability and accuracy of the characteristic quantity value, can be rapidly disintegrated in cold water by utilizing the characteristics of the apple high-sugar matrix without adding auxiliary materials such as an adhesive and a lubricant, and removes the acid source and the alkali source in a manner of forming salt through an acid-alkali reaction and dissolving the salt in water; the influence of matrix difference caused by auxiliary materials on a laboratory detection result is avoided.
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Description

Technical Field

[0001] The present application relates to the field of pesticide residue detection and element analysis, and in particular to a quality control effervescent tablet for pesticide residue and metal element determination, and a preparation method and application thereof. Background Art

[0002] Food safety has always been the focus of attention of all sectors of society and the general public. Its scientific evaluation basis is accurate test data. The common international practice is to implement matrix quality control sample testing and evaluation simultaneously during the testing process, so as to ensure the accuracy of the data while avoiding the influence of matrix effects on the test results.

[0003] At present, commercial fruit matrix quality control samples sold on the market are mostly preserved in the form of fruit puree or freeze-dried powder. Fruit puree is easy to spoil, has a short shelf life, needs to be frozen for storage, and needs to be thawed before use. Frequent thawing can easily cause uneven matrix, thus affecting the accuracy of characteristic values. In order to solve the problem of fruit puree being difficult to preserve, the more common method is to freeze-dry the fruit, crush it and make it into fruit freeze-dried powder, which can retain the original matrix of the fruit to the maximum extent after removing the water.

[0004] Most common fruits such as apples, oranges, and bananas have a sugar content greater than 10%, and the sugar content of freeze-dried matrices is even higher. Existing studies have shown that the temperature at which a high-sugar matrix changes from a glassy state to a rubbery state is relatively low. When the matrix is ​​in a glassy state, all aspects of its properties are very stable; when the matrix changes from a glassy state to a rubbery state, its physical and chemical properties such as structure, texture, microbial activity, and enzyme activity change, and the apparent phenomenon is agglomeration. Since many properties of the high-sugar matrix have changed after agglomeration and the water content has increased, the characteristic values ​​and their uncertainties determined in the early stage of the quality control sample have a significant impact.

[0005] Chinese patent document CN116754546A discloses a cholinesterase effervescent tablet for detecting pesticide residues, a preparation method and a use method. By making acetylcholinesterase into an effervescent tablet by embedding and granulating, the rate of decrease of its activity at room temperature is delayed. Chinese patent document CN116421660A discloses a Jinpuju effervescent tablet for treating wind-heat attacking the lungs in upper respiratory tract infection, which is used to treat wind-heat attacking the lungs in upper respiratory tract infection. Chinese patent document CN115836715A discloses an Actinidia arguta effervescent tablet with anti-fatigue effect and a preparation method thereof. This invention can solve the problem of Actinidia arguta being difficult to store for a long time to the greatest extent.

[0006] However, there is no report on the preparation method of quality control sample effervescent tablets for pesticide residue and metal element detection in the above prior art. In addition, after using the prior art to prepare effervescent tablets for pesticide residue detection and element analysis, the accuracy of the analysis results is affected due to the matrix effect caused by the large amount of auxiliary materials. Summary of the invention

[0007] The present invention aims to overcome the problem that the effervescent tablets in the prior art are not applicable to the field of pesticide residue and metal element detection. Therefore, a quality control effervescent tablet for pesticide residue and metal element determination and a preparation method thereof are provided to overcome the above-mentioned shortcomings.

[0008] To achieve the above-mentioned purpose, the present invention is implemented by the following technical solutions: In a first aspect, the present invention first provides a quality control effervescent tablet for the determination of pesticide residues and metal elements. It is prepared by mixing and tableting the spiked sample and disintegrant; The spiked sample includes freeze-dried fruit and vegetable powder and standard substances added inside the fruit and vegetable powder for detecting pesticides and metal elements; the freeze-dried fruit and vegetable powder contains greater than or equal to 45% fructose, and the total sugar content in the freeze-dried fruit and vegetable powder is greater than or equal to 60%; The particle size of the freeze-dried fruit and vegetable powder is less than or equal to the particle size of the disintegrant.

[0009] As described in the background technology, existing commercially available fruit matrix quality control samples are mostly stored in the form of fruit puree or freeze-dried powder. Both forms of quality control samples are inconvenient to use and difficult to store. The quality control sample in this application is in the form of an effervescent tablet, which can ensure the stability and accuracy of the characteristic value while being convenient for laboratory use. It is an innovation in the preparation of laboratory quality control samples and has huge economic and social benefits.

[0010] However, in the prior art, the effervescent tablet is usually prepared by first preparing acid granules and alkali granules from the acid source and alkali source in the disintegrant, and then the acid granules, alkali granules and the target material are mixed and compounded and then pressed to form an effervescent tablet. In this process, it is usually necessary to add a certain amount of adhesive (such as polyvinyl pyrrolidone, polyvinyl alcohol) and lubricant, so as to meet the final tablet with a certain fastness and not easily broken. However, the addition of adhesive and lubricant will have a certain impact in the qualitative and quantitative analysis of pesticide residue detection and metal element process, thereby affecting the accuracy of the test data.

[0011] Therefore, in the process of preparing quality control effervescent tablets for pesticide residue and metal element determination, we should avoid adding exogenous adhesives to prevent the interference of adhesives on the test results. Compared with the effervescent tablets in the prior art, the quality control effervescent tablets in the present application can form quality control effervescent tablets without exogenous interference by simply mixing and tableting the two components of spiked samples and disintegrants during the preparation process. Since the quality control effervescent tablets in the present application do not add auxiliary materials such as adhesives and lubricants, while rapidly disintegrating, the influence of matrix differences caused by excipients on laboratory test results is avoided.

[0012] However, after mixing and tableting different types of spiked samples with pure disintegrants, the inventors of the present application found that the appearance of the quality control effervescent tablets obtained by pressing different types of spiked samples under the same ratio and tableting conditions was extremely different. Among them, some spiked samples were loose and brittle after pressing, and some samples could not even be tableted. Therefore, mixing and pressing spiked samples with pure disintegrants is not as easy as originally imagined.

[0013] Therefore, the inventor of the present application has conducted in-depth research on this issue. The results show that there are usually three different forms of sugars, fructose, glucose and sucrose, in fruits and vegetables, and the distribution ratios of the three are different in different fruits and vegetables. Through research, it is found that among the three sugars in fruits and vegetables, the content of fructose has a significant effect on the bonding stability of the quality control effervescent tablets, so that we can control the fructose content in the freeze-dried fruit and vegetable powder to make the structure of the quality control effervescent tablets obtained by tableting more compact, making the quality control effervescent tablets less likely to absorb water, so that the quality control effervescent tablets can still meet the quality control requirements after long-term storage. However, the glucose and sucrose in fruits and vegetables have no significant effect on the tableting effect of the quality control effervescent tablets.

[0014] In addition to the fructose content in the freeze-dried fruit and vegetable powder having a significant effect on the tableting effect, the inventors of the present application also found that the particle size ratio between the freeze-dried fruit and vegetable powder and the disintegrant also has a significant effect on the tableting effect. When the particle size difference between the freeze-dried fruit and vegetable powder used as a binder and the disintegrant is too large, it will also affect the inherent viscosity of the fructose inside the freeze-dried fruit and vegetable powder, thereby affecting the final tablet fastness.

[0015] Preferably, the preparation method of the spiked sample is as follows: a) Collect fruits and vegetables from the same batch, discard inedible parts, chop into pieces, and grind into a pulp; b) adding the pesticide and metal element standard substances evenly into the fruit and vegetable pulp, and freeze-drying and dehydrating the pulp; c) taking the dried block sample, crushing it into powder by a grinder and further mixing it to obtain the spiked sample.

[0016] Preferably, the method for preparing the spiked sample further comprises the step of adding fructose to the spiked sample.

[0017] Preferably, the freeze-drying conditions in step b) are as follows: pre-freezing temperature -40°C to -5°C, pre-freezing time 1 to 6 hours, cold trap temperature -196°C to -20°C, freezing time 30 minutes to 96 hours.

[0018] Preferably, the standard substance of the pesticide is any one or more of cyhalothrin, deltamethrin, bifenthrin, chlorpyrifos, and thiophanate-methyl. The standard substance of the metal element is a compound containing any one or more elements of lead, mercury, cadmium, antimony, manganese, nickel and aluminum.

[0019] Preferably, the mass ratio of the spiked sample to the disintegrant is (60%-80%):(40%-20%).

[0020] Preferably, the disintegrant comprises an acid source and an alkali source, and the ratio of the acid source to the alkali source is 1:(1-1.6).

[0021] In a second aspect, the present invention also provides a method for preparing the quality control sample effervescent tablet, comprising the following steps: (1) uniformly mixing the spiked sample and the disintegrant to obtain a mixed material; (2) tabletting the mixture to obtain the quality control sample effervescent tablet.

[0022] In a third aspect, the present invention also provides the use of the quality control sample effervescent tablet as described above in detecting the content of pesticides and metal elements in agricultural and sideline products.

[0023] Therefore, the present invention has the following beneficial effects: The present invention utilizes the inherent characteristics of the high-sugar matrix of apples, does not add auxiliary materials such as adhesives and lubricants, can quickly disintegrate in cold water, removes acid and alkali sources by forming salts through acid-base reactions and dissolving in water, and avoids the influence of matrix differences caused by auxiliary materials on laboratory test results.

[0024] The present invention adopts the form of tablets, which is convenient for laboratory use while ensuring the stability and accuracy of characteristic values. It is an innovation in laboratory quality control sample preparation and has huge economic and social benefits. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 These are photos of the film-forming effects of Comparative Examples 1-4.

[0026] Figure 2 These are photos of quality control effervescent tablets obtained by pressing different varieties of fruit and vegetable powders.

[0027] Figure 3 These are photos of quality control effervescent tablets obtained by pressing lemon powder with different fructose addition amounts.

[0028] Figure 4 These are photos of quality control effervescent tablets obtained by pressing fruit and vegetable powders with different particle sizes and disintegrants. DETAILED DESCRIPTION

[0029] The present invention is further described below in conjunction with specific embodiments. Those of ordinary skill in the art will be able to implement the present invention based on these descriptions. In addition, the embodiments of the present invention involved in the following description are generally only embodiments of a part of the present invention, rather than all embodiments. Therefore, based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative work should fall within the scope of protection of the present invention.

[0030] [Preparation Example]: Preparation example of disintegrant ratio in effervescent tablets Preparation Example 1: A quality control sample effervescent tablet for determination of pesticide residues and metal elements in apple powder is obtained by the following steps: Step A: discard the core and stalk of the apple matrix, take the pulp part, chop the required sample into small pieces with a knife, grind it into a paste with a fruit and vegetable grinder, add a mixed standard methanol solution of five pesticides (methyl thiophanate, chlorflucythrin, deltamethrin, bifenthrin, chlorpyrifos) and a standard aqueous solution of a metal element (lead) and mix well to obtain spiked apple puree, and pack the spiked apple puree in a freezing plate (filling thickness 5mm) and put it into a freeze dryer for freeze drying and dehydration to obtain spiked apple powder. The spiked apple powder is crushed again through a 35-mesh sieve (500μm) and then put into a mixer at 50 rpm and mixed for 12 hours to obtain spiked apple powder for preparing effervescent tablets.

[0031] Step B: According to the proportion of 1.0g of apple powder (the moisture content of apple is about 90%, which is about 10g after re-dissolving in equal proportion, which is consistent with the sampling amount of the existing standard detection method in my country), 0.57g of sodium bicarbonate and 0.43g of citric acid, the effervescent tablets are made by direct tableting.

[0032] Preparation Example 2-5: Preparation Examples 2-5 and Preparation Example 1 use the same spiked apple powder, the difference being the difference in the proportion of disintegrants (sodium bicarbonate and citric acid), see Table 1 below for details.

[0033] Table 1: Proportion of disintegrant in Preparation Examples 1-5 Film effect evaluation Physical appearance evaluation: observe the regularity and fastness of the finished product.

[0034] Evaluation of disintegration effect: Take 1 tablet, place it in a 50mL centrifuge tube, add 9mL of water (20℃±5℃), measure its disintegration time, and observe the intensity of the reaction and the final disintegration state.

[0035] result: Five tablets prepared by direct compression with different mixing ratios were tested. Preparation Examples 1-5 all experienced disintegration reactions to varying degrees. In Preparation Example 1, there was too much disintegrant, the acid-base reaction was violent, and the foam escaped from the centrifuge tube, resulting in the loss of the apple powder reference material. In Preparation Example 5, there was too little disintegrant, the acid-base reaction was too slow, and the apple powder agglomerated in the water and could not be completely disintegrated. The disintegration results are detailed in Table 2. According to the experimental results, the disintegration effect of Preparation Example 3 (70% apple powder reference material and 30% disintegrant) was the most ideal.

[0036] Table 2: Evaluation of tableting effect of Preparation Examples 1-5 Preparation example of acid-base ratio in disintegrant: Preparation Example 6-10: According to the results of the previous apple powder reference material and disintegrant ratio, under the condition of the optimal apple powder to disintegrant ratio of 7:3, the total amount of disintegrant was fixed at 0.428g. Preparation Examples 6-10 used the same spiked apple powder as Preparation Example 1, the difference being the difference in the ratio of sodium bicarbonate and citric acid in the disintegrant, as shown in Table 3 below.

[0037] Table 3: Acid-base ratio in disintegrants Tableting effect evaluation Five preparation examples with different acid-base ratios were tested. Preparation examples 6-10 all had different degrees of disintegration reactions, among which preparation examples 6 and 10 almost did not disintegrate; preparation examples 7 and 9 did not disintegrate completely; preparation example 8 had the best disintegration effect, and the results are shown in Table 4.

[0038] Table 4: Tablet disintegration effects of 5 different acid-base mixtures name Disintegration time Disintegration effect Preparation Example 6 >3min Almost no disintegration Preparation Example 7 >3min Incomplete disintegration Preparation Example 8 <3min Complete disintegration Preparation Example 9 >3min Incomplete disintegration Preparation Example 10 >3min Almost no disintegration Comparative example of effervescent tablet preparation process: Comparative Example 1 Citric acid and sodium bicarbonate were passed through a 35-mesh sieve to obtain acid particles (citric acid) and alkali particles (sodium bicarbonate). 2g of 5% anhydrous ethanol PVP (polyvinyl pyrrolidone) solution was added to 20g of acid particles and alkali particles in batches as a binder, and after being stirred and mixed evenly, the mixture was granulated through a 20-mesh sieve, dried in a 50°C oven for 50min, and then passed through a 20-mesh sieve for standby use. According to the proportion of 1.0g of apple powder (same as Preparation Example 1), 0.596g of sodium bicarbonate (containing a binder) and 0.450g of citric acid (containing a binder), semi-dry granules were used for tableting to prepare effervescent tablets.

[0039] Comparative Examples 2-4 Comparative Examples 2-4 adopt the same preparation process as Comparative Example 1, the difference being the difference in the proportion of disintegrants (sodium bicarbonate and citric acid), as shown in Table 5 below.

[0040] Table 5: Ratio of apple powder reference material to disintegrant (semi-dry granulation tableting method) Tableting effect evaluation Comparative Example 1 can be tableted, but the tablet edge is rough, the texture is loose and fragile, and the uneven distribution of apple powder and disintegrant can be clearly observed; Comparative Examples 2-4 have soft texture, low fastness, and are fragile, and cannot be tableted. Figure 1 The main reason is that the particle size of the granular acid and granular base prepared by the semi-dry granulation method is larger than that of the apple powder reference material, which reduces the inherent viscosity of the apple powder and affects the final sheet fastness.

[0041] Preparation examples of different types of fruits and vegetables First, the fructose content and total sugar content in different fruit and vegetable powders were determined, and then the same preparation method as in Preparation Example 1 was used to prepare effervescent tablets from fruits and vegetables with different fructose contents.

[0042] The sugar content of different types of fruits and vegetables is shown in Table 6 below.

[0043] Table 6 Determination results of sugar content in fruits and vegetables fructose(%) glucose(%) sucrose(%) Total sugar (%) Apple powder 46.9 22.1 8.03 77.0 Banana powder 15.2 15.0 32.5 62.7 Lemon Powder 0.78 1.37 0.48 2.6 Papaya powder 1.20 1.87 0.00 3.1 Celery Powder 2.10 0.00 0.00 2.1 Cucumber powder 7.76 18.00 0.75 26.5 The evaluation results of the effects of fruit and vegetable slices with different fructose contents are shown in Table 7 below.

[0044] Table 7: Evaluation of the effect of fruit and vegetable slices with different fructose contents From the results in Table 7, we can see that the fructose content in the freeze-dried fruit and vegetable powder has a significant effect on the tableting effect. When the native fructose content in the freeze-dried fruit and vegetable powder is high (Preparation Example 1), the quality control sample effervescent tablet obtained by tableting has a high physical appearance, and the tablets are usually uniform and regular round tablets with clear edges and a certain degree of fastness; however, after tableting fruits and vegetables with low fructose content (Preparation Example 11, Preparation Example 12, Preparation Example 13), it was found that tablets could not be formed. The photos of the fruit and vegetable powders with different fructose contents after tableting are shown in the figure. Figure 2 However, when a certain amount of fructose was added to the fruit (lemon powder) with low fructose content (Preparation Examples 14-20), it was found that the tableting effect was improved with the increase of fructose addition, which proved that fructose content has a positive effect on the tableting effect. The photos of lemon powder with different fructose additions after tableting are shown in the figure. Figure 3 As shown. Moreover, with the increase of fructose content, the tableting effect of fruit powder effervescent tablets is getting better and better. When the fructose content accounts for more than 60% of the main material, the effervescent tablets can be pressed into tablets. It can be seen that fructose has a bonding effect, which is consistent with the conclusion that the high fructose content in apple powder has a good self-bonding effect. The reason is that fructose itself has good hygroscopicity, which affects its tableting effect. Only when the content of externally added fructose accounts for more than 60% of the main material can it play a good bonding role in the experimental system designed this time.

[0045] Preparation examples of different particle size ratios between freeze-dried fruit and vegetable powders and disintegrants The same preparation method as in Preparation Example 1 was used to compound apple powders with different particle sizes and disintegrants (sodium bicarbonate and citric acid) with different particle sizes to obtain effervescent tablets. For details, see Table 8 and Figure 4 .

[0046] Table 8: Evaluation of tableting effect of different particle size ratios between freeze-dried fruit and vegetable powder and disintegrant From Table 8 and Figure 4 The results show that the relationship between the particle size of the fruit and vegetable powder and the particle size of the disintegrant in the effervescent tablet has a significant impact on the quality of the effervescent tablet. Generally speaking, when the particle size of the disintegrant is smaller than that of the fruit and vegetable powder, the tablet quality is better, and when the particle size of the disintegrant is larger than the mass of the fruit and vegetable powder, it will cause difficulty in demolding the tablet, resulting in fragmentation failure during demolding.

[0047] [Experimental example]: Experimental instruments: Gas chromatography-tandem mass spectrometer: Agilent 7890 / 7000D; liquid chromatography-mass spectrometer: Agilent1290 / 9490; inductively coupled plasma mass spectrometer: Agilent 8900.

[0048] Standards and Reagents Nitric acid, methanol, and acetonitrile were all of mass spectrometry grade (Thermo Scientific). Ultrapure water used for sample treatment and chromatographic mobile phase was from Milli-Q ultrapure water system (Millipore Corporation). Standards were purchased from the National Institute of Metrology, China.

[0049] Experimental Example 1: Basis for evaluating uniformity of quality control effervescent tablets The quality control sample effervescent tablets prepared this time were divided into about 200 tablets. According to the provisions of JJF 1343-2022 "Value determination and uniformity and stability evaluation of reference materials", 11 samples were randomly selected and the measurement variance between samples (S1 2 ) and an independent estimate of measurement repeatability (S2 2 ) were compared to verify the homogeneity of the samples.

[0050] Evaluation of the uniformity of quality control effervescent tablets The detection of cyhalothrin, deltamethrin, bifenthrin and chlorpyrifos is based on GB 23200.113-2018 "Determination of 208 pesticides and their metabolites in plant-derived foods by gas chromatography-tandem mass spectrometry", the detection of methyl thiophanate is based on GB / T 20769-2008 "Determination of 450 pesticides and related chemicals in fruits and vegetables by liquid chromatography-tandem mass spectrometry", and the detection of lead is based on GB 5009.268-2016 "National Food Safety Standard Determination of Multiple Elements in Food". The extracted samples were pre-treated and instrumentally analyzed. The uniformity statistics show that the statistical values ​​F are all less than the F critical value (F α )2.91, through the F test, the statistics and results are shown in Table 9 below.

[0051] Table 9: Evaluation of uniformity of quality control effervescent tablets Experimental Example 2: Basis for stability evaluation of quality control effervescent tablets According to JJF 1343-2022 "General Principles and Statistical Principles for the Determination of Reference Materials", the stability assessment is carried out at -18°C to examine the influence of temperature on the characteristic values ​​in the quality control effervescent tablets.

[0052] Stability evaluation of quality control effervescent tablets Randomly select samples from the prepared quality control effervescent tablets and store them in a freezer (about -18°C) for 0, 7, 14, 30, 60 and 90 days, with 6 samples selected each time. According to the t-test, after being stored in a freezer (about -18°C) for 0, 7, 14, 30, 60 and 90 days, the t values ​​of each group were less than the critical value t(0.95,10) =1.8125, all passed the t-test, see Table 10-15 for details.

[0053] Table 10: Statistical results of cyhalothrin stability Table 11: Statistical results of stability of cypermethrin Table 12: Statistical results of the stability of bifenthrin Table 13: Statistical results of chlorpyrifos stability Table 14: Statistical results of thiophanate-methyl stability Table 15: Statistical results of lead stability Experimental Example 3: Comparison of test results of quality control effervescent tablets and spiked apple powder Six samples were randomly selected from the prepared quality control effervescent tablets, and six samples were spiked with apple powder. The samples were pre-treated and instrumentally analyzed. After t-test, the t values ​​of each group were less than the critical value t( 0.95,10 )=1.8125, all passed the t-test. The specific results are shown in Tables 16-21.

[0054] Table 16: Statistical results of cyhalothrin Table 17: Statistical results of cypermethrin Table 18: Statistical results of bifenthrin Table 19: Statistical results of chlorpyrifos Table 20: Statistical results of methyl thiophanate Table 21: Lead statistics results The specific embodiments described herein are merely examples of the spirit of the present invention. A person skilled in the art of the present invention may make various modifications or additions to the specific embodiments described or replace them in a similar manner, but this will not deviate from the spirit of the present invention or exceed the scope defined by the appended claims.

Claims

1. A quality control effervescent tablet for the determination of pesticide residues and metal elements, characterized in that: It is prepared by mixing and tableting the spiked sample and disintegrant; The spiked samples include freeze-dried fruit and vegetable powder and standard substances added into the fruit and vegetable powder for detecting pesticides and metal elements; The freeze-dried fruit and vegetable powder contains greater than or equal to 45% fructose, and the total sugar content in the freeze-dried fruit and vegetable powder is greater than or equal to 60%.

2. A quality control effervescent tablet for determination of pesticide residues and metal elements according to claim 1, characterized in that: The particle size of the freeze-dried fruit and vegetable powder is less than or equal to the particle size of the disintegrant.

3. A quality control effervescent tablet for determination of pesticide residues and metal elements according to claim 1 or 2, characterized in that: The preparation method of the spiked sample is as follows: a) Collect fruits and vegetables from the same batch, discard inedible parts, chop into pieces, and grind into a pulp; b) adding the pesticide and metal element standard substances evenly into the fruit and vegetable pulp, and freeze-drying and dehydrating the pulp; c) taking the dried block sample, crushing it into powder by a grinder and further mixing it to obtain the spiked sample.

4. A quality control effervescent tablet for determination of pesticide residues and metal elements according to claim 3, characterized in that: The method for preparing the spiked sample further comprises the step of adding fructose to the spiked sample.

5. A quality control effervescent tablet for determination of pesticide residues and metal elements according to claim 3, characterized in that: The freeze-drying conditions in step b) are as follows: pre-freezing temperature -40°C to -5°C, pre-freezing time 1 to 6 hours, cold trap temperature -196°C to -20°C, freezing time 30 minutes to 96 hours.

6. A quality control effervescent tablet for determination of pesticide residues and metal elements according to any one of claims 1 to 5, characterized in that: The standard substance of the pesticide is any one or more combinations of cyhalothrin, deltamethrin, bifenthrin, chlorpyrifos, and thiophanate-methyl; The standard substance of the metal element is a compound containing any one or more elements of lead, mercury, cadmium, antimony, manganese, nickel and aluminum.

7. A quality control effervescent tablet for determination of pesticide residues and metal elements according to claim 1, characterized in that: The mass ratio of the spiked sample to the disintegrant is (60%-80%):(40%-20%).

8. A quality control effervescent tablet for determination of pesticide residues and metal elements according to claim 1 or 7, characterized in that: The disintegrant comprises an acid source and an alkali source, and the ratio of the acid source to the alkali source is 1:(1-1.6).

9. A method for preparing a quality control sample effervescent tablet as claimed in any one of claims 1 to 8, characterized in that: The following steps are involved: (1) uniformly mixing the spiked sample and the disintegrant to obtain a mixed material; (2) tabletting the mixture to obtain the quality control sample effervescent tablet.

10. Use of the quality control effervescent tablet according to any one of claims 1 to 8 in detecting the content of pesticides and metal elements in agricultural and sideline products.

Citation Information

Patent Citations

  • Actinidia arguta effervescent tablet with anti-fatigue effect and preparation method of actinidia arguta effervescent tablet

    CN115836715A

  • Trichosanthes kirilowii maxim effervescent tablet for treating wind-heat affecting lung disease of upper respiratory tract infection

    CN116421660A

  • Cholinesterase effervescent tablet for detecting pesticide residues and preparation method and use method thereof

    CN116754546A