CN100595555C - Analytic sample of animal drug residue in meat powder and preparation process thereof - Google Patents
Analytic sample of animal drug residue in meat powder and preparation process thereof Download PDFInfo
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- CN100595555C CN100595555C CN200610046391A CN200610046391A CN100595555C CN 100595555 C CN100595555 C CN 100595555C CN 200610046391 A CN200610046391 A CN 200610046391A CN 200610046391 A CN200610046391 A CN 200610046391A CN 100595555 C CN100595555 C CN 100595555C
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Abstract
This invention relates to an analytic sample of animal drug residue in meat powder and preparation process thereof<0}. With veterinary medicine content in 0.001~1000mg/kg, the preparation process comprises: selecting fresh meat, removing tendon to mince, adding medicine, homogenizing, vacuum freezing out, breaking into pieces for sieving, and packing to protect against damp. This invention needs low cost, benefit to stabilize veterinary medicine, damages little to original ingredients, contains little water in frozen powder for package and storage in long time, and has high yield.
Description
Affiliated field:
That the present invention relates to is digested tankage veterinary drug residue analytic sample and preparation technology thereof, particularly adopts the method for the digested tankage veterinary drug residue analytic sample of vacuum freeze drying technology preparation.
Background technology:
Residue of veterinary drug (veterinary drug residue) is meant that the parent, metabolic product of the contained veterinary drug of any edible part of animal product and the impurity relevant with veterinary drug are residual, is called for short " medicine is residual ".Do not observe the off-drug period regulation, illegally to use forbidden drug, Irrational Use of Drugs etc. be the main cause that causes residue of veterinary drug.At present, main residual animal medicine has antibiotics, sulfamido, furans, steroids, anticoccidial class and drives insect medicine.
Along with global economic integration and food trade internationalization, food security has become the important public health problem of a global challenge and the whole world, and its veterinary drug residue problem is to influence food, one of key factor of esp meat goods edible safety.The poisoning that residue of veterinary drug in the meat products causes human body, allergic reaction and teratogenesis, mutagenesis and effect serious harm such as carcinogenic consumers in general healthy, in addition, residue of veterinary drug has also caused very big threat to aquaculture, food processing industry and food trade etc., and there is potentiality harm in environment, finally influence human existence safety.So meat products veterinary drug residue problem has caused global extensive concern, countries in the world are actively developed this type of residual testing one after another.
For the quality assurance of testing, the normal method that adopts of common laboratory includes laboratory internal soundness control, as selection standard material or the sample that is similar to standard substance quality management and instrumental correction is carried out in testing.In addition, also include between the laboratory test result comparison, as by the domestic breadboard proficiency testing of CNAL (CNAL) tissue with by the proficiency testing of the International Laboratory of Asia-Pacific Laboratory Accreditation committee orgaization.Proficiency testing is one of important evidence of relevant approval council evaluation experimental chamber technical capability, is to judge and the effective means of monitoring experiment chamber ability, and the while also is to keep one of basis that international accreditation body recognizes each other.No matter be the sample of controlling as the laboratory internal soundness, still as the proficiency testing test sample, their common features will stablize exactly, evenly, and then effectively the monitoring experiment chamber interior detects quality, also can be in proficiency testing, the result who reports by the laboratory of respectively participating in the experiment provides correctly, rational evaluation, relatively reaches judgement its detectability situation.
Vacuum freeze drying technology originates from the twenties in 19th century, after the fluctuating of having experienced decades and pacing up and down, makes significant progress in last 20 years.Enter 21 century, vacuum freeze drying technology relies on the incomparable advantage of other drying means, more and more be subjected to people's favor, the goods made from this technology often possess do not change ultimate constituent, easily store, be difficult for going mouldy, advantage such as long shelf-life, so be widely used in fields such as medicine, biological products, food, blood product, active substance, but this technology is applied to the quality control of preparation experiment chamber interior sample, especially detection of veterinary drugs in food quality control sample and proficiency testing with the still rarely seen at home report of sample.The present invention introduces the residue of veterinary drug analysis field with vacuum freeze drying technology, and be prepared into the digested tankage analytic sample of animal drug residue, this sample empirical tests has good properties, needs can be satisfied, also it due effect can be brought into play as general analytic sample in the routine work of laboratory in addition as laboratory internal soundness control sample and proficiency testing specimen.This invention has not only been opened up a new technical field for the preparation of analytic sample of animal drug residue, has promoted the exploitation of retention analysis sample, and also to improving the quality of retention analysis sample, the kind of enriching the retention analysis sample has positive effect.
Summary of the invention:
The purpose of this invention is to provide a kind of digested tankage veterinary drug residue analytic sample and preparation technology thereof, this method has that technology is simple, cost is low, easy to operate, veterinary drug is evenly distributed, stablize, freeze-dried powder does not destroy ultimate constituent, easily preservation, long shelf-life, yield rate advantages of higher.Digested tankage veterinary drug residue analytic sample of the present invention can be used for general detecting, test result comparison etc. between the control of laboratory internal soundness and laboratory.
Digested tankage veterinary drug residue analytic sample comprises digested tankage and veterinary drug, and the veterinary drug content range in the described digested tankage is at 0.001～1000mg/Kg.
The granularity of described digested tankage veterinary drug residue analytic sample is 20～200 orders.
The meat of described preparation digested tankage is meats such as beef, pork, mutton, donkey meat, rabbit meat, dog meats, chicken, duck, goose.
Described veterinary drug is Du-6859as such as Enrofloxacin, Ciprofloxacin, Pefloxacin, first Flucloxacillin, Norfloxacin, Lomefloxacin, gatifloxacin, Ofloxacin, Enoxacin; Furans medicines such as furazolidone, furaltadone, nitrofurazone, furans benzene olefin(e) acid sodium, furantoin, nitrofurazone; Sulfonamides such as sulphadiazine, sulfametoxydiazine, sulfadimidine, sulfaquinoxaline; Tri-Biocins such as penicillin, terramycin, tetracycline, streptomysin, erythromycin, chloromycetin, ovobiocin; Amcinonides such as diethylstilbestrol, estradiol, norethindrone, CA; Anthelmintics such as levamisol, trichloro-benzenes azoles, doractin, closantel; Anticoccidial drugs such as Metichlorpindol, diclazuril, toltrazuril, dinitolmide, Nicarbazin; Hematozoon such as Diminazene Aceturate, Sha Molin medicine; Anthelmintics such as Fenbendazole, albendazole, Oxibendazole, oxfendazole, albendazole; And beta-stimulants such as its woods of the female Te Luo of Clenbuterol, Zilpaterol, ripple Lip river, western sieve Bart, Ke Lunpante, tulobuterol, salbutamol, special cloth, spray Boot sieve, fenoterol, betaxolol, inderal.
A kind of preparation method of digested tankage veterinary drug residue analytic sample is characterized in that may further comprise the steps:
A. select; B. rub; C. add veterinary drug; D. be mixed; E. freeze-drying; F. sieve; G. pack.
Fresh meat is selected → is gone muscle rubbing → interpolation veterinary drug → homogenate and is mixed → vacuum freeze-drying → crushing screening → damp-prrof packing.
Described vacuum freeze-drying comprises pre-freeze and two processes of vacuum drying.The pre-freeze temperature is controlled at-10～-100 ℃, and vacuum drying vacuum degree control is at 0.0001～10000Pa, and freeze temperature is controlled at-100～80 ℃, and the finished product water cut can reach 0.5～10%.
The digested tankage veterinary drug residue analytic sample of this method preparation has following advantage: technology is simple, cost is low, easy to operate.Fresh meat is easy to mix with veterinary drug after rubbing, and in pre-freeze and process of vacuum drying, veterinary drug is in ultralow temperature or the vacuum state all the time, helps the stable of veterinary drug; Dry under the condition of low temperature and vacuum, ultimate constituent is not destroyed substantially; The fresh meat sample becomes minimum particle through homogenized before the freeze-drying, be easy to the later stage pulverize, and during freeze-drying moisture directly to distil be gas, the composition of solid does not change, the yield rate height; Only contain a spot of water in the freeze-dried powder,, be convenient to preserve, and be difficult for going mouldy, so but long-term storage so the branch packing is carried out in visual requirement.
Embodiment:
Processing process:
Embodiment 1: the preparation of enrofloxacin residual analytic sample in the powdered beef
(1) selects, select the about 10kg of neat, the fresh beef of outward appearance;
(2) go muscle to rub, remove muscle, put in the meat grinder and rub;
(3) add Enrofloxacin, get the bright beef 8kg after the rubbing, stir, add Enrofloxacin 0.5mg, stir;
(4) homogenate is mixed, and the above-mentioned sample that mixes is all poured into homogenate in the refiner, is mixed;
(5) vacuum freeze-drying is slowly poured the above-mentioned sample that mixes in the freeze-drying dish, again the freeze-drying dish is put into vacuum freeze-drier ,-20 ℃ of pre-freezes, after this keeps the interior vacuum tightness of freeze-drier 10
4Below the Pa, freeze temperature rises to 20 ℃ gradually from-20 ℃, vacuumizes, drying, treats that water cut reaches at about 5% o'clock, takes out, and sample places closed container to keep in Dark Place; Vacuum freeze-drier is selected FD-1 type freeze dryer for use;
(6) crushing screening places comminutor to pulverize in the freeze-drying sample, and sieves, and gets the sieve low-grades, and product granularity is 60 orders, and the veterinary drug amount that contains of product is 62.5mg/Kg;
(7) damp-prrof packing adopts the wrappage of good airproof performance to pack, and prevents the moisture absorption.
Embodiment 2: the preparation of Metichlorpindol retention analysis sample in the chicken meal
(1) fresh meat is selected, and selects neat, the fresh chicken 5Kg of outward appearance;
(2) go muscle to rub, remove muscle, put in the meat grinder and rub;
(3) add Metichlorpindol, get and rub the about 4Kg of back fresh chicken meat, stir, add Metichlorpindol 0.1mg, stir;
(4) homogenate is mixed, and the above-mentioned sample that mixes is all poured into homogenate in the refiner, is mixed;
(5) vacuum freeze-drying is slowly poured the above-mentioned sample that mixes in the freeze-drying dish, again the freeze-drying dish is put into vacuum freeze-drier ,-20 ℃ of pre-freezes, after this keeps the interior vacuum tightness of freeze-drier 10
4Below the Pa, freeze temperature rises to 10 ℃ gradually from-20 ℃, vacuumizes, drying, treats that water cut reaches at about 5% o'clock, takes out, and sample places closed container to preserve; Vacuum freeze-drier is selected FD-1 type freeze dryer for use;
(6) crushing screening places comminutor to pulverize in the freeze-drying sample, and sieves, and gets the sieve low-grades, and product granularity is 60 orders, and the veterinary drug amount that contains of product is 2.5mg/Kg;
(7) damp-prrof packing adopts the wrappage of good airproof performance to pack.
Claims (4)
1, a kind of preparation method of digested tankage veterinary drug residue analytic sample is characterized in that the preparation method may further comprise the steps: fresh meat is selected → is gone muscle rubbing → interpolation veterinary drug → homogenate and is mixed → vacuum freeze-drying → crushing screening → damp-prrof packing.
2, the preparation method of digested tankage veterinary drug residue analytic sample according to claim 1 is characterized in that described vacuum freeze-drying comprises pre-freeze and two processes of vacuum drying; The pre-freeze temperature is controlled at-10～-100 ℃, and vacuum drying vacuum degree control is at 0.0001～10000Pa, and freeze temperature is controlled at-100～80 ℃, and the finished product water cut can reach 0.5～10%.
3, the preparation method of digested tankage veterinary drug residue analytic sample according to claim 1 is characterized in that the preparation of enrofloxacin residual analytic sample in the powdered beef:
(1) selects: select the about 10kg of neat, the fresh beef of outward appearance;
(2) go muscle to rub: to remove muscle, put in the meat grinder and rub;
(3) add Enrofloxacin: get the bright beef 8kg after the rubbing, stir, add Enrofloxacin 0.5mg, stir;
(4) homogenate is mixed: the above-mentioned sample that mixes is all poured into homogenate in the refiner, is mixed;
(5) vacuum freeze-drying: the above-mentioned sample that mixes is slowly poured in the freeze-drying dish, again the freeze-drying dish is put into vacuum freeze-drier,-20 ℃ of pre-freezes, after this keep the interior vacuum tightness of freeze-drier below 104Pa, freeze temperature rises to 20 ℃ gradually from-20 ℃, vacuumizes, drying, treats that water cut reaches at about 5% o'clock, take out, sample places closed container to keep in Dark Place;
(6) crushing screening: the meat pie that freeze-drying is good places comminutor to pulverize, and sieves, and gets the sieve low-grades, and product granularity is 60 orders, and the veterinary drug amount that contains of product is 62.5mg/Kg;
(7) damp-prrof packing: adopt the wrappage of good airproof performance to pack, prevent the moisture absorption.
4, the preparation method of digested tankage veterinary drug residue analytic sample according to claim 1 is characterized in that the preparation of Metichlorpindol retention analysis sample in the chicken meal:
(1) fresh meat is selected: select neat, the fresh chicken 5Kg of outward appearance;
(2) go muscle to rub: to remove muscle, put in the meat grinder and rub;
(3) add Metichlorpindol: get the about 4Kg of fresh chicken meat after the rubbing, stir, adding Metichlorpindol 0.1mg stirs;
(4) homogenate is mixed: the above-mentioned sample that mixes is all poured into homogenate in the refiner, is mixed;
(5) vacuum freeze-drying: the above-mentioned sample that mixes is slowly poured in the freeze-drying dish, again the freeze-drying dish is put into vacuum freeze-drier,, after this keep the interior vacuum tightness of freeze-drier 10-20 ℃ of pre-freezes
4Below the Pa, freeze temperature rises to 10 ℃ gradually from-20 ℃, vacuumizes, drying, treats that water cut reaches at about 5% o'clock, takes out, and sample places closed container to preserve;
(6) crushing screening: the meat pie that freeze-drying is good places comminutor to pulverize, and sieves, and gets the sieve low-grades, and product granularity is 60 orders, and the veterinary drug amount that contains of product is 2.5mg/Kg;
(7) damp-prrof packing: adopt the wrappage of good airproof performance to pack.
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| CN200610046391A CN100595555C (en) | 2006-04-19 | 2006-04-19 | Analytic sample of animal drug residue in meat powder and preparation process thereof |
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| CN200610046391A CN100595555C (en) | 2006-04-19 | 2006-04-19 | Analytic sample of animal drug residue in meat powder and preparation process thereof |
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Cited By (1)
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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 |
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| CN103293039A (en) * | 2013-05-30 | 2013-09-11 | 福建出入境检验检疫局检验检疫技术中心 | Method for quickly obtaining positive material containing AOZ (3-amino-2-oxazolidinone) minced shrimp natural matrix in laboratory |
| CN104155163B (en) * | 2014-08-22 | 2015-10-28 | 威海出入境检验检疫局检验检疫技术中心 | Toltrazuril in chicken, ponazuril remain the method for making of freeze-dried powder standard model |
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| CN109613148A (en) * | 2019-01-30 | 2019-04-12 | 中国水产科学研究院黄海水产研究所 | The preparation method of AOZ residue criterion substance turbot muscle as matrix |
| CN110672754A (en) * | 2019-11-13 | 2020-01-10 | 贵州省兽药饲料监察所(贵州省兽药残留监测中心) | Method for determining nicarbazin content in feed |
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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 |
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