CN100359315C - Animal remedy residual ability verification sample and method for preparing same - Google Patents
Animal remedy residual ability verification sample and method for preparing same Download PDFInfo
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- CN100359315C CN100359315C CNB2005100465368A CN200510046536A CN100359315C CN 100359315 C CN100359315 C CN 100359315C CN B2005100465368 A CNB2005100465368 A CN B2005100465368A CN 200510046536 A CN200510046536 A CN 200510046536A CN 100359315 C CN100359315 C CN 100359315C
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Abstract
The present invention relates to an animal remedy residue ability verification sample which belongs to the field of ability verification. Animal remedies are added to a base material until the content of the animal remedies reaches 50 ppb to 5 ppm, wherein the base material is selected from animal livers as food sources; the animal remedies are tetracyclines, chloramphenicol, or sulphonamides, etc. Compared with the prior art, the present invention has the advantages that the selection of the base material is scientific and reasonable, a preparation method is mature and reliable, micro quantities and even trace quantities of animal remedies can be distributed uniformly into substances to be measured, and the successful rate of sample preparation is high. By the present invention, ability verification samples for transport and transmission at normal temperature can be prepared, the residue content of animal remedies contained in the samples approaches to that of animal remedies contained in actual samples and is uniform and stable enough to meet the requirements of ability verification.
Description
Technical field
The present invention relates to the sample in the ability verification in proficiency testing specimen preparation field, particularly residue of veterinary drug and the preparation method of sample.
Background technology
In order to guarantee the safe and sanitary of livestock products, prevent and monitor animal derived food Chinese traditional medicine and poisonous and harmful substance are residual, improve the quality of China's animal product, ensure people's health.The proficiency testing project that carry out in domestic food physics and chemistry field focuses mostly in early days in the analysis of nutritional labeling, as albumen, the analysis of fat, in recent years, the food additives in the beverage have also been organized, methyl alcohol in the drinks, aflatoxin in the peanut, the proficiency testing of projects such as the tetracycline in the honey is residual (or claiming horizontal checkout), but the mechanism that does not have the ripe food physical and chemical testing proficiency testing project of a cover, be difficult to the effectively breadboard detectability of checking food safety detection, be difficult to accuracy, reliability and the authority of objective appraisal laboratory detection result.Proficiency testing is to utilize the laboratory detection result comparison to determine a kind of activity of laboratory detectability.The common requirement of proficiency testing sample is that sufficiently high homogeneity and stability will be arranged, and the singularity of detection of veterinary drugs in food is that residue of veterinary drug is trace or even trace in animal body, how on this contents level, to prepare uniform sample, be difficult to realize.
Summary of the invention
The objective of the invention is to overcome above-mentioned not whole problem, a kind of animal remedy residual ability verification sample is provided, content is near actual residue, but the normal temperature transportation, and homogeneity stability all can reach the proficiency testing requirement.Its preparation method also is provided in addition, can be distributed to the veterinary drug of trace or even trace in the test substance equably and removes specimen preparation success ratio height.
The technical scheme that the present invention is adopted for achieving the above object is: animal remedy residual ability verification sample, and adding veterinary drug to veterinary drug content in the matrix is 50ppb-5ppm, matrix is food source property animal's liver.
Described matrix is chicken gizzard, pork liver, beef liver, sheep liver.Veterinary drug is veterinary drugs such as telracycline family, chloromycetin or sulfamido, particularly is selected from any kind in sulfamido veterinary drug sulphadiazine, sulfadimidine, sulfanilamide (SN) 5-Sulfamonomethoxine, sulfadimethoxine or the sulfaquinoxaline.
Choice of base of the present invention is scientific and reasonable, sulfamido is as prevention and medicine for treatment and be widely used in the edible animal, its residual each organ that also is distributed in animal body, as skin. fat. muscle. internal organ etc., and in some internal organs generation enrichment, so many countries have also stipulated maximum residue limit(MRL) in different tissues to sulfa drugs.Remaining in of sulfa drugs is higher than anti-its hetero-organization that waits of its hetero-organization muscle fat in liver and the kidney.In the residual Supervisory Surveillance Program of China, be mostly that the sulfa drug residue in the liver (as chicken gizzard, pork liver, beef liver, sheep liver etc.) to animal is monitored.The sample of proficiency testing usually should be similar with participate in the experiment breadboard daily detection article or material in nature, so we select the liver of animal as detected material.Research shows that sheep liver powder and chicken gizzard powder are the preferable detected materials as detection of veterinary drugs in food by experiment.
The preparation method of animal remedy residual ability verification sample of the present invention:
1, matrix pre-service: will eat source property animal's liver and clean, remove impurity, do not contain kind residue of veterinary drug to be measured after testing after, adopt freeze-drying or boulton process drying, dried liver is ground to granularity less than 80 orders through pulverizing, and makes blank hepar siccatum;
2, preparation sample: adopt the solvent distribution, elder generation is dissolved in veterinary drug in the solvent and mixes, and more blank hepar siccatum is immersed in the solution, fully mixes, after the solvent evaporates, pulverize, grind, fully mixing, cross 80 orders with top sieve, sealing, refrigerated storage promptly gets animal remedy residual ability verification sample;
Wherein solvent is chosen the solvent that meets following three kinds of conditions simultaneously: the solubleness of a. veterinary drug in solvent is good; B. veterinary drug does not change in solvent; C. solvent volatility is good.Solvent is methyl alcohol and acetonitrile preferably.
Described solvent load is that the blank hepar siccatum consumption of every gram is the 2-4ml solvent.
Described solvent evaporates adopts nitrogen to dry up, and during to fast doing, moves into vacuum drying chamber, is evaporated to driedly, in the whole process, constantly stirs, and keeps temperature 20-40 degree, example weight to be obtained and blank hepar siccatum weight near the time, solvent evaporates is complete.
The present invention compared with prior art, have the following advantages and beneficial effect: matrix is selected rationally, method for making is simple and reliable, can be distributed to the veterinary drug of trace or even trace in the test substance equably and go, adopting the present invention to prepare can be for normal temperature transportation and the proficiency testing sample that transmits, approaching in residue of veterinary drug content that is contained and the actual sample, enough all even stable, satisfy the proficiency testing requirement.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment 1:
Agents useful for same and standard substance:
Water: ultrapure water, methyl alcohol: chromatographically pure, acetonitrile: chromatographically pure, chloroform: chromatographically pure
Sulphadiazine: Riedel-de Haen, 99.9%, CAS-Nr:68-35-9
Sulfadimidine: Riedel-de Haen, 99.7%, CAS-Nr:57-68-1
Sulfanilamide (SN) 5-Sulfamonomethoxine: Riedel-de Haen, 99.8%, CAS-Nr:651-06-9
Sulfadimethoxine: Riedel-de Haen, 99.9%, CAS-Nr:122-11-2
Sulfaquinoxaline: Sigma, 95%, CAS-Nr:59-40-5
1, the matrix pre-service: commercially available sheep liver (chicken gizzard) is through cleaning, remove impurity (for preventing the error that the host material difference is brought to sample homogeneity, should remove all fat as far as possible, blood vessel, manadesma etc., only keep the liver entity), after adopting the detection of liquid phase method or liquid matter method not contain five kinds of sulfamido residues of veterinary drug to be measured, adopt freeze-drying or boulton process drying, baking temperature 20-40 ℃, prevent the too high protein denaturation that causes of temperature, dried sheep liver (chicken gizzard) is through pulverizing, be ground to granularity less than 80 orders (a part of dried hepar siccatum granularity after grinding can not reach discarding below 80 orders), make blank sheep liver (chicken gizzard) powder.
2, specimen preparation: sample size weighing blank sheep liver (chicken gizzard) the powder 1000g definite according to laboratory quantity and the statistics design of participating in the experiment, the veterinary drug that accurate again weighing is added: sulphadiazine 1-2mg, sulfadimidine 1-2mg, sulfanilamide (SN) 5-Sulfamonomethoxine 1-2mg, sulfadimethoxine 2-4mg, sulfaquinoxaline 2-4mg, veterinary drug is dissolved in the q.s 100ml methyl alcohol, mix, pour in sheep liver (chicken gizzard) powder, fully mix, be placed in wealthy mouthful and the shallow container, dry up with nitrogen, during to fast doing, move into vacuum drying chamber, be evaporated to dried.In the whole process, need to stir frequently, and keep temperature not to be higher than 40 degree.Sheep liver (chicken gizzard) grain weight amount to be obtained and initial sheep liver (chicken gizzard) grain weight amount near the time, can think that the methyl alcohol evaporation is fully in the sample.After the taking-up, pulverize, grind, fully mixing is crossed 80 mesh sieves, and sealing, refrigerated storage are standby, and this duplicate samples hereinafter is called full-page proof.
Full-page proof above is tiled on the clean free of contamination worktable, the underlay Polypropylence Sheet, quadrate, with glass bar equidistant each three line anyhow that draw, full-page proof is divided into 16 equal lattice, from different grid, take out sample, pack into and distribute in the vial of sample, weighing is to predetermined weight (expectation is distributed to the breadboard example weight of participating in the experiment, and is each sample 4.0 gram in the works at T036), seal with sealer, random number, adhesive label, record number, lucifuge-18 ℃ freezing preservation hereinafter is called sample.
Properties of sample to preparation is tested:
1, sample homogeneity test:
Sample: the sheep liver powder that has added sulfamido veterinary drug to be measured.
Instrument and equipment: Agilent1100 high performance liquid chromatograph, band UV-detector.
Supercentrifuge, homogenizer, ultrasonic oscillation device, balance, Nitrogen evaporator
Reagent and medicine: acetonitrile: chromatographically pure.Chloroform: chromatographically pure.Acetate: top grade is pure.
Normal hexane: chromatographically pure.
Chromatographic condition: chromatographic column: COSMOSIL, 5C18-Mr, 4.6*250mm.
Moving phase: 0.3% acetic acid aqueous solution+acetonitrile, gradient elution.
Flow velocity: 0.9ml/min.
UV-detector detects wavelength: 280nm.
Method: from the proficiency testing sample for preparing, randomly draw 12 uniformity test samples.Each uniformity test sample is made two parallel samples (A and B) respectively; Adopt SN0208-93 to carry out sample pre-treatments (comprise and extract and purify) and test; But all tests must be carried out two experiments under repeat condition, as same laboratory, and same personnel, same quadrat method, same equipment is finished test in the short as far as possible time.The statistical procedures of homogeneity data.
The test gained the results are shown in Table 1.1 and table 1.2.
Table 1.1 sample A homogeneity experimental result
Table 1.1 sample A homogeneity experimental result (continuing)
Table 1.1 sample A homogeneity experimental result (continuing)
Table 1.1 sample A homogeneity experimental result (continuing)
Table 1.1 sample A homogeneity experimental result (continuing)
Table 1.2 sample B homogeneity experimental result
Table 1.2 sample B homogeneity experimental result (continuing)
Table 1.2 sample B homogeneity experimental result (continuing)
Table 1.2 sample B homogeneity experimental result (continuing)
Table 1.2 sample B homogeneity experimental result (continuing)
2, sample stability test
Sample is positioned over preserves the detection of carrying out project to be measured behind the certain hour under the environmental baseline that may experience after sending,, transmit in the sample transportation with research, in the test process, whether its project to be measured marked change takes place.Be used for guaranteeing to participate in the experiment the laboratory after receiving sample,, just can not produce outlier because stability of sample is bad as long as in proficiency testing plan official hour, finish detection.International proficiency testing is difficult to accomplish the sample refrigeration transportation in the works, and sample is under the normal temperature condition substantially.At present under the traffic condition, external laboratory needs to receive in 7-10 days sample, domestic laboratory needs to receive in 2-7 days sample, sample of the present invention has carried out 60 days stability experiments of room temperature, the sample of wherein considering will be through the equator in transmittance process, the sample that has laboratory (south) environment temperature of participating in the experiment when detecting is higher, and the time sample retention temperature in one of them week is at 30 ℃-35 ℃.
Sample: from each the proficiency testing sample for preparing, randomly draw 12 stability test samples.Be placed on room temperature preservation in the exsiccator.
Instrument and equipment, reagent and medicine and chromatographic condition detect used identical with homogeneity.
Method: from exsiccator, randomly drawed 3 stability test samples every 10 days.Each stability test sample is divided into two parallel samples, detects respectively.The statistical procedures gained experimental data of stability data sees Table 2.
Table 2 sample stability experimental result
Conclusion: prove by sample homogeneity and 60 days stability experiments, the resulting proficiency testing sample of above described proficiency testing sample preparation methods can satisfy the requirement of animal remedy residual ability verification plan, and the appearance of outlier is all enough got well and can not cause to its homogeneity and stability.The solvent distribution of this research innovation is effective in the preparation of animal remedy residual ability verification solid-state normal-temperature sample, can promote the use of in the preparation of food physics and chemistry detectability verification sample (solid-state, normal temperature).
Claims (8)
1, animal remedy residual ability verification sample is characterized in that: make in the matrix by following preparation method that to add veterinary drug content be the sample of 50ppb-5ppm:
(1), the matrix pre-service: matrix is eaten source property animal's liver cleans, remove impurity, do not contain kind residue of veterinary drug to be measured after testing after, adopt freeze-drying or boulton process drying, dried liver is ground to granularity less than 80 orders through pulverizing, and makes blank hepar siccatum;
(2), preparation sample: adopt the solvent distribution, elder generation is dissolved in veterinary drug in the solvent and mixes, and more blank hepar siccatum is immersed in the solution, fully mixes, after the solvent evaporates, pulverize, grind, fully mixing is crossed the following sieve of 80 orders, and sealing, refrigerated storage promptly get animal remedy residual ability verification sample;
Wherein solvent is chosen the solvent that meets following three kinds of conditions simultaneously: the solubleness of a. veterinary drug in solvent is good; B. veterinary drug does not change in solvent; C. solvent volatility is good.
2, animal remedy residual ability verification sample according to claim 1 is characterized in that: matrix is chicken gizzard, pork liver, beef liver, sheep liver.
3, animal remedy residual ability verification sample according to claim 1 is characterized in that: veterinary drug is microbiotic, chloromycetin or sulfamido veterinary drug.
4, animal remedy residual ability verification sample according to claim 1 is characterized in that: veterinary drug is any kind that is selected from sulfamido veterinary drug sulphadiazine, sulfadimidine, sulfanilamide (SN) 5-Sulfamonomethoxine, sulfadimethoxine or the sulfaquinoxaline.
5, according to the preparation method of the arbitrary described animal remedy residual ability verification sample of claim 1-4, it is characterized in that:
(1), the matrix pre-service: will eat source property animal's liver and clean, remove impurity, do not contain kind residue of veterinary drug to be measured after testing after, adopt freeze-drying or boulton process drying, dried liver is ground to granularity less than 80 orders through pulverizing, and makes blank hepar siccatum;
(2), preparation sample: adopt the solvent distribution, elder generation is dissolved in veterinary drug in the solvent and mixes, and more blank hepar siccatum is immersed in the solution, fully mixes, after the solvent evaporates, pulverize, grind, fully mixing is crossed the following sieve of 80 orders, and sealing, refrigerated storage promptly get animal remedy residual ability verification sample;
Wherein solvent is chosen the solvent that meets following three kinds of conditions simultaneously: the solubleness of a. veterinary drug in solvent is good; B. veterinary drug does not change in solvent; C. solvent volatility is good.
6, the preparation method of animal remedy residual ability verification sample according to claim 5 is characterized in that: solvent is methyl alcohol and acetonitrile.
7, according to the preparation method of claim 5 or 6 described animal remedy residual ability verification samples, it is characterized in that: solvent load is that the blank hepar siccatum consumption of every gram is the 2-4ml solvent.
8, the preparation method of animal remedy residual ability verification sample according to claim 5, it is characterized in that: solvent evaporates adopts nitrogen to dry up, during to fast doing, move into vacuum drying chamber, be evaporated to dried, in the whole process, constantly stir, keep temperature 20-40 degree, example weight to be obtained and blank hepar siccatum weight near the time, solvent evaporates is complete.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101290306B (en) * | 2008-06-18 | 2011-11-02 | 内蒙古蒙牛乳业（集团）股份有限公司 | Milk and milk product tetracycline antibiotic residual quantity checking method |
| CN106596216A (en) * | 2015-11-02 | 2017-04-26 | 中国检验检疫科学研究院 | Veterinary drug residual quantity verification sample containing sulfamethazine and preparation method thereof |
| CN109187136A (en) * | 2018-09-19 | 2019-01-11 | 上海市疾病预防控制中心 | A kind of preparation method and application applied to laboratory pesticide residue proficiency testing sample |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106596215A (en) * | 2015-11-02 | 2017-04-26 | 中国检验检疫科学研究院 | Proficiency testing sample of furaltadone metabolite-containing veterinary drug residue and preparation method thereof |
| CN106323718A (en) * | 2016-11-04 | 2017-01-11 | 辽宁省检验检疫科学技术研究院 | Standard sample of chloramphenicol, thiamphenicol and fluorine thiamphenicol in pork, preparation method and application |
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| WO2002008241A2 (en) * | 2000-07-21 | 2002-01-31 | Gilead Sciences, Inc. | Prodrugs of phosphonate nucleotide analogues and methods for selecting and making same |
| CN1547013A (en) * | 2003-12-08 | 2004-11-17 | 中国农业大学 | Enzyme linked immuno kit for detecting sulfadimidine |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101290306B (en) * | 2008-06-18 | 2011-11-02 | 内蒙古蒙牛乳业（集团）股份有限公司 | Milk and milk product tetracycline antibiotic residual quantity checking method |
| CN106596216A (en) * | 2015-11-02 | 2017-04-26 | 中国检验检疫科学研究院 | Veterinary drug residual quantity verification sample containing sulfamethazine and preparation method thereof |
| CN109187136A (en) * | 2018-09-19 | 2019-01-11 | 上海市疾病预防控制中心 | A kind of preparation method and application applied to laboratory pesticide residue proficiency testing sample |
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