CN106813963A - A kind of fish powder standard substance preparation method containing chloramphenicol - Google Patents
A kind of fish powder standard substance preparation method containing chloramphenicol Download PDFInfo
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- CN106813963A CN106813963A CN201710117226.3A CN201710117226A CN106813963A CN 106813963 A CN106813963 A CN 106813963A CN 201710117226 A CN201710117226 A CN 201710117226A CN 106813963 A CN106813963 A CN 106813963A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
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Abstract
The invention discloses a kind of fish powder standard substance preparation method containing chloramphenicol.Fed by simulating, the fish material of chloramphenicol pollution is obtained, is homogenized after in appropriate proportions mixing with water after sample pretreatment, the lyophilized flesh of fish is obtained using freeze-drying method, by steps such as grinding, screening, mixing, irradiation, the lyophilized fish meal with excellent homogeneity is prepared.Uniformity testing and STABILITY MONITORING are carried out with the high accuracy measurement of liquid chromatogram isotope dilution mass spectrometry, and standard substance assignment.Lyophilized fish meal containing trace amount chloramphenicol prepared by this method, uniformity and has good stability, and can be used for evaluation, the quality control of analysis process and the laboratory capabilities examination of chloramphenicol trace residue analysis method in aquatic products.Calibration measurement utensil is can also be used for as standard substance and evaluate measuring method.
Description
Technical field
The present invention relates to a kind of fish powder substrate standard substance preparation method containing trace amount chloramphenicol, chlorine is mould in fish powder
Plain standard substance is a kind of measurement criteria, is mainly used in calibration measurement utensil and evaluates the degree of accuracy of measuring method.
Background technology
Chloramphenicol (chloramphenicol, CAP), scientific name D- Su Shi-(-)-N- [α-(hydroxymethyl)-beta-hydroxy-right
Nitrophenethyl] -2,2- dichloro acetamides, molecular formula is C11H12Cl2N2O5, needle-like, the length of white needles or micro-strip yellow green
Flaky crystal or crystalline powder, 149-153 DEG C of fusing point, 19.5 DEG C of specific rotatory power, water solubility is 2.5g/L.Soluble in water and first
Alcohol, ethanol, acetone, propane diols etc..No. CAS is 56-75-7, molecular weight 323.1294.Chemical structural formula is as shown in Figure 1.
Chloramphenicol is a kind of high-efficiency broad spectrum antibiotic, is widely applied in terms of animal infectious disease preventing and treating.But
It is that the chloramphenicol remained in edible animal can be enriched with by food chain in human body, to health composition potential hazard.European Union, the U.S.
Chloramphenicol is classified as legal disabling veterinary drug, European Union determines that minimum limitation is 0.3 μ g/kg, and China also specifies in animal food
Chloramphenicol " must not be detected ".Gas chromatography-mass spectrography or LC/MS (LC-MS) are that current chloramphenicol is detected most
Main confirmation method.But the characteristics of due to Mass Spectrometer Method, requires that the pre-treatment of sample and purification process are complicated, mainly includes that chlorine is mould
Plain extractions, protein removal, impurity purification, concentration, the process such as filter and cause that analysis cost is high, flux is low, it is even more important that
Pretreatment process, condition control, matrix effect of very complicated etc. have impact on reliability and the degree of accuracy of testing result, document report
The liquid chromatograph mass spectrography in road or the result relative standard deviation (RSD) of gas chromatography-mass spectrography method typically exist
Between 20%~35%, the judgement of the result near Limited Doses is directly affects.
For trace amount chloramphenicol residue detection result has traceability, comparativity and accuracy in ensureing aquatic products, need badly open
Exhibition has accurate assignment, the development of chloramphenicol standard substance in uniform, stabilization the flesh of fish.The successful development of the standard substance can
Ensure the flesh of fish in chloramphenicol measurement result accurately and reliably, and then have to ensuring food safety extremely important social benefit and
Economic benefit.
The content of the invention
The present invention provides a kind of fish powder standard substance preparation method containing chloramphenicol.It is an object of the invention to provide one
The fish powder standard substance containing trace amount chloramphenicol is planted, with good uniformity and stability.The use of the standard substance has
Beneficial to the Matrix Match degree of chloramphenicol trace residue detection Plays material and sample in the flesh of fish is improved, so as to improve detection knot
The accuracy and reliability of fruit.
The present invention also provides a kind of preparation method of the fish powder substrate standard substance containing chloramphenicol, including：
Sample pretreatment：The flesh of fish is rejected into fishbone and fish-skin, manadesma, stripping and slicing is rubbed, as raw material；Take raw material appropriate, press
According to 1:3 ratio, is diluted with water into meat slurry, using 5000rpm, low-temperature and high-speed homogeneous 3min, homogenate 10 times is repeated, per minor tick
30min；Homogenate loads refrigerator tray；Thickness of sample is no more than 2cm in the refrigerator tray.
Pre-freeze sample：The sample eutectic point is -15 DEG C, sets pre-freezing temperature and is set to -20 DEG C；Pre-freeze speed be 10 DEG C/
min；Quick pre-freeze 2 hours；
First stage lyophilization：The refrigerator tray is loaded into dry case, after dry case pressure more normal time-preserving, with
The speed of 5 DEG C/time steps up shelf temperature, until -5 DEG C；When sample temperature rise to it is true close to shelf temperature or dry case
When reciprocal of duty cycle is approached and keep constant with cold-trap vacuum, continue to dry 1 hour；
Second stage lyophilization：Below 0-4 DEG C of the maximum temperature that once adjustment shelf temperature to sample is allowed；It is automatic to adjust
Section permeation, the time is on 2 hours；After sample reaches maximum permissible temperature, recover vacuum, constant temperature 4 hours in dry case；
Grinding flour：Lyophilized sample is ground in grinder, grinding rate is 3000rpm, grind 1min；
Screening：Using 35 mesh sieves, ultrasonic pulse screening sample；
Mix：Sample is placed in 10L mixing buckets, continuous to mix 6 hours；
Obtain fish powder substrate standard substance.
Packing：Sample packaging 15mL transparent samples bottle in, every bottle of about 2.5g；
Irradiation：The gamma-rays produced using radio isotope cobalt -60, radiation sterilizing, irradiation dose are carried out to freeze-dried powder
It is 4kGy.
The present invention compared with other technologies, it is advantageous that：1) after in appropriate proportions mixing with water after sample pretreatment
Homogenate, using the lyophilized flesh of fish of freeze-drying method acquisition, by steps such as grinding, screening, mixing, irradiation, preparing has
The lyophilized fish meal of excellent homogeneity.2) fed by simulating, obtain the fish material of chloramphenicol pollution, the raw material being capable of mould completely
Chloramphenicol pollution flesh of fish sample during plan is actually detected；3) contents level (0.6 μ of chloramphenicol in fish meal is prepared using the technology
G/kg) with the minimum residue limits level of European Union (0.3 μ g/kg) in an order of magnitude, the need for meeting trace residue detection.
Lyophilized fish meal containing chloramphenicol prepared by the method that the present invention is provided, uniformity and has good stability, and can be used for
The evaluation of analysis method, the quality control of analysis process and laboratory capabilities are examined during chloramphenicol trace residue is detected in aquatic products
Core.Also can simultaneously be used for calibration measurement utensil as standard substance and evaluate measuring method, it is simple to operate, it is easy to promote.
Other features and advantages of the present invention will be illustrated in the following description, also, the partly change from specification
Obtain it is clear that or being understood by implementing the present invention.The purpose of the present invention and other advantages can be by the explanations write
Specifically noted structure is realized and obtained in book, Figure of description, claims.
Below in conjunction with the accompanying drawings, by embodiment, technical scheme is described in further detail.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, with reality of the invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is chloramphenicol molecular structure；
Fig. 2 is the MRM detection spectrograms of the chloramphenicol LC-MSMS of fish meal sample.
Specific embodiment
The preferred embodiments of the present invention are illustrated below, it will be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
In the present embodiment, it is necessary first to obtain raw material, that is, the flesh of fish sample containing chloramphenicol.
Standard substance candidate is obtained by the way of feeding.Purchase Tilapia mossambica, it is ensured that feeding water and fish jar used
Chloramphenicol is not contained, after blank is raised two weeks, Preliminary detection, it is determined that the flesh of fish is blank sample.According to doses in water body
In add chloramphenicol, repeat addition chloramphenicol after water body is changed weekly, it is continuous to raise 6 weeks.
1st, sample pretreatment is oppressed：
(1) positive Tilapia mossambica is taken, fishbone and fish-skin, manadesma etc. is rejected, stripping and slicing is rubbed, as raw material.
(2) raw material is taken appropriate, according to 1:3 ratio, is diluted with water into meat slurry, using 5000rpm, low-temperature and high-speed homogeneous
3min, repeats homogenate 10 times (per minor tick 30min).
(3) homogenate loads refrigerator tray (30cm*30cm*5cm), and thickness of sample is no more than 2cm in disk.
2nd, prepared by flesh of fish freeze-dried powder：
(1) pre-freeze sample：Sample eutectic point is -15 DEG C, sets pre-freezing temperature and is set to -20 DEG C；Pre-freeze speed be 10 DEG C/
Min (11 DEG C of cooling per minute)；Quick pre-freeze 2 hours, makes sample freeze jail completely.
(2) first stage lyophilization：
After pre-freeze is terminated, start first stage distillation.After dry case pressure more normal time-preserving, with the speed of 5 DEG C/time
Rate steps up shelf temperature, until -5 DEG C, prevent sample from supercooling occur, for distillation provides energy, accelerate rate of sublimation.
Approached with cold-trap vacuum and keep constant when sample temperature is risen to close to shelf temperature or dry case vacuum
When, continue to dry 1 hour, thoroughly to eliminate the lack of uniformity of the residual ice crystal in sample and sample drying, first stage distillation
Terminate.
(3) second stage lyophilization
Do not exist in the stage sample and freezed ice, once adjusted 0-4 DEG C of the maximum temperature that shelf temperature to sample is allowed
Below.To avoid hypotony influence heat transfer in dry case, automatically adjust permeation, so that sample temperature reaches the highest temperature as early as possible
Degree, improves rate of sublimation.Time is on 2 hours.
After sample reaches maximum permissible temperature, recover vacuum, constant temperature 4 hours, second stage lyophilization knot in dry case
Beam.
(4) shut down, take out lyophilized sample.Weigh, freeze-dried powder yield is 23%.
3rd, grinding flour：Lyophilized sample grinds in grinder, and grinding rate is 3000rpm, grinds 1-2min.
4th, sieve：Using 35 mesh sieves, ultrasonic pulse screening sample.
5th, mix：Sample is placed in 10L and mixes in bucket (no more than the 1/2 of bucket volume), continuous to mix 6 hours.
6th, dispense：Sample packaging 15mL transparent samples bottle in, every bottle of about 2.5g.
7th, irradiate：The gamma-rays produced using radio isotope cobalt -60, radiation sterilizing is carried out to freeze-dried powder, irradiates agent
It is 4kGy to measure.
Lyophilized fish meal sample to trace amount chloramphenicol obtained in the above method carries out uniformity testing and STABILITY MONITORING.
(1) uniformity testing
Uniformity is the base attribute of standard substance, for the spatial distribution characteristic of description standard substance characteristics.In standard
Uniformity assessment must be carried out during the development (production) of material, to prove that it has good uniformity.
The detection method of uniformity：
Pre-treatment：Weigh flesh of fish 2g.10mL 0.1mol sodium acetate buffers (pH=5), vortex 2min are added, then is added
Enter 20mL ethyl acetate, vortex 1min, mechanical shaking extraction 15min, 5000r/min refrigerated centrifuge (4 DEG C) 5min collects 15mL acetic acid
In ethyl ester extract solution to 15mL centrifuge tubes.Oasis PRIME HLB posts are directly crossed, after collecting eluent, the nitrogen under 45 DEG C of water-baths
Air-blowing is done, and residue is mixed with 1ml15% methanol-waters, crosses 0.22 μm of GHP filter membrane, is determined for LC/MS/MS.
Instrumental Analysis：AB-QTRAP 5500；Chromatographic column：ACQUITY CSHTM C18, 1.7 μm, 3.0 × 100mm；Column temperature：
40℃；Sample size：10μL；Mobile phase：A phases：The acetic acid of water+0.1%；B phases：Methyl alcohol；Flow velocity is 0.3ml/min.Other mobile phases
Condition is shown in Table 1.
Table 1 other mobile phase conditions
| Time(Time) | 0.01 | 1 | 3 | 3.01 | 5 | 5.01 | 8 |
| Pump B | 15 | 70 | 70 | 90 | 90 | 15 | Stop |
Mass Spectrometry Conditions：Anion scan mode；Many reflections monitoring (MRM)；Electron spray voltage (IS)：-4500V；Gas curtain gas
Pressure (CUR)：15psi；Atomization gas pressure (GS1)：55psi；Assist gas pressure power (GS2)：50psi；Ion source temperature：550℃；
Qualitative ion pair, quota ion pair, go cluster voltage (DP), collision cell entrance potential (EP), collision cell exit potential (CXP) and
The condition of collision gas energy (CE) is shown in Table 2.
The chloramphenicol quantitative and qualitative ion pair of table 2 and mass spectrum relevant operating parameter
Randomly select 15 packagings from 300 of standard substance packagings, each pack take 3 increments carry out bottle between and bottle
Interior uniformity testing.Minimum sample mass is 0.5g, according to liquid chromatogram isotope dilution mass spectrometry (LC-IDMS/ as described below
MS) tested.By uniformity the results of analysis of variance sbbWith the repeated s of method thereforrOr the characteristic magnitude uncertainty
Target is compared, if not significantly, standard substance is considered as uniformly.The inhomogeneities that characteristic magnitude to be measured should be calculated is introduced
Partial uncertainty ubb, and counted the total uncertainty of standard substance.Standard substance is carried out according to the method described above
Uniformity testing, uniformity testing the results are shown in Table 3.
The uniformity testing result of table 3
The estimate of standard deviation is calculated with following formula between bottle：
Repeatability standard deviation srS can be used2 2Calculate：
Result finds sbb>sr, therefore uniformity standard deviation s between bottlebb=ubb=0.0164 μ g/kg.This standard material is uniform
Property introduce uncertainty be 0.0164 μ g/kg
(2) Detection of Stability
Stability is the base attribute of standard substance, for the property that the characteristic magnitude of description standard material is changed over time
Matter, the i.e. Time-distribution of description standard substance characteristics.Stability assessment must be carried out in the development process of standard substance.
Stability assessment can not only assess the uncertainty of measurement related to stability of material, and can specify suitable storage and transport
Condition.
For this standard material, the method for taking the stability of synchronization to assess, by first close rear thin principle, is investigated and protected in regulation
Deposit under condition (0-4 DEG C), the stability of sample after preserving 0,1,2,3,6 months.Enter according to foregoing LC-MS method
Row test, takes 5 packagings every time, and each packaging takes an increment, surveys 3 times, calculates average value, 5 measurement results of packaging
Average value is used as testing result.The STABILITY MONITORING data of standard substance are calculated using trend analysis method, and evaluates steady
The uncertainty of qualitative introducing, is stablized in definite value result range of uncertainty using the variation of result as criterion material
Principle.Due to can truly describe the mechanism of degradation of chloramphenicol in fish meal without physically or chemically model, therefore can select linear
Model as the candidate criteria material empirical model.Stability evaluation result is shown in Table 4, and stability is introduced not as seen from table
It is defined as 0.0114ug/kg.
The long-time stability of chloramphenicol and trend analysis (t=6 month) in the fish meal of table 4
(3) definite value
Chloramphenicol substrate standard substance in fish meal, using liquid chromatogram isotopic dilution tandem mass spectrum Par value, system is ground
Study carefully method, sample pre-treatments, testing conditions etc., and use Duo Jia laboratory cooperation definite values.
For chloramphenicol standard substance in the fish meal of preparation, using liquid chromatogram isotope dilution mass spectrometry Duo Jia laboratories
Cooperation definite value.With reference to ISO directive/guides 34：2000《The General Requirement of standard substance producer's ability》Managerial ability to partner,
The aspect such as technical capability and hardware facility proposes to be distinctly claimed to the laboratory for participating in cooperation definite value.Selection 8 is satisfactory
Collaboration laboratory.
Cooperation definite value requires that 8 groups of data are tested in each laboratory to each standard substance, for all test datas point
Equal precision measurement differentiation is not carried out and outlier is rejected.
Meet normal distribution through Xia Piluo-welker's method inspection determination data.
Definite value result is as shown in table 5.
The definite value result of table 5
Definite value result：The standard value of chloramphenicol standard substance is 0.601 μ g/kg in fish meal, and uncertainty is 0.043 μ g/
kg。
As shown in Fig. 2 for the MRM of the chloramphenicol LC-MS/MS of fish meal sample detects spectrogram.
In sum, the lyophilized fish meal containing chloramphenicol that prepared by this method, uniformity and has good stability, and can be used for water
The evaluation of analysis method, the quality control for analyzing process and laboratory capabilities examination in the detection of chloramphenicol trace residue in product.
Also can simultaneously be used for calibration measurement utensil as standard substance and evaluate measuring method, it is simple to operate, it is easy to promote.
Obviously, those skilled in the art can carry out various changes and modification without deviating from essence of the invention to the present invention
God and scope.So, if these modifications of the invention and modification belong to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising these changes and modification.
Claims (3)
1. a kind of fish powder standard substance preparation method containing chloramphenicol, it is characterised in that including：
Sample pretreatment：The flesh of fish that chloramphenicol is polluted rejects fishbone and fish-skin, manadesma, and stripping and slicing is rubbed, as raw material；Take original
Material is appropriate, according to 1:3 ratio, is diluted with water into meat slurry, using 5000rpm, low-temperature and high-speed homogeneous 3min, repeats homogenate 10
It is secondary, per minor tick 30min；Homogenate loads refrigerator tray；
Pre-freeze sample：The sample eutectic point is -15 DEG C, sets pre-freezing temperature and is set to -20 DEG C；Pre-freeze speed is 10 DEG C/min；
Quick pre-freeze 2 hours；
First stage lyophilization：The refrigerator tray is loaded into dry case, after dry case pressure more normal time-preserving, with 5 DEG C/
Secondary speed steps up shelf temperature, until -5 DEG C；Sample temperature rise to close to shelf temperature or dry case vacuum with
When cold-trap vacuum is approached and keeps constant, continue to dry 1 hour；
Second stage lyophilization：Below 0-4 DEG C of the maximum temperature that once adjustment shelf temperature to sample is allowed；Automatically adjust and ooze
Gas, the time is on 2 hours；After sample reaches maximum permissible temperature, recover vacuum, constant temperature 4 hours in dry case；
Grinding flour：Lyophilized sample is ground in grinder, grinding rate is 3000rpm, grind 1min；
Screening：Using 35 mesh sieves, ultrasonic pulse screening sample；
Mix：Sample is placed in 10L mixing buckets, continuous to mix 6 hours；
Obtain fish powder substrate standard substance.
2. the method for claim 1, it is characterised in that methods described also includes：
Thickness of sample is no more than 2cm in the refrigerator tray.
3. the method for claim 1, it is characterised in that methods described also includes：
Irradiation：The gamma-rays produced using radio isotope cobalt -60, radiation sterilizing is carried out to freeze-dried powder, and irradiation dose is
4kGy。
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107319271A (en) * | 2017-08-16 | 2017-11-07 | 江门华大生物科技有限公司 | A kind of irradiation-induced degradation method of aquatic products antibiotic |
| CN107478478A (en) * | 2017-08-08 | 2017-12-15 | 上海市农业科学院 | A kind of fumonisin B1Substrate standard substance and preparation method thereof |
| CN108387416A (en) * | 2018-02-01 | 2018-08-10 | 辽宁出入境检验检疫局检验检疫技术中心 | Methyl mercury residue detection standard sample and preparation method thereof in shark meat |
| CN108663467A (en) * | 2018-06-21 | 2018-10-16 | 马长征 | A kind of preparation method of fish meal Analysis on amino acid components standard substance |
| 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 |
| 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 |
| CN111610073A (en) * | 2020-05-26 | 2020-09-01 | 云南省计量测试技术研究院 | Preparation method of heavy metal-containing Yunnan pseudo-ginseng standard substance |
| CN112649271A (en) * | 2020-11-18 | 2021-04-13 | 嘉兴浙华食品健康研究有限公司 | Preparation method of milk powder standard substance containing aflatoxin AFTM1 |
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| CN107478478A (en) * | 2017-08-08 | 2017-12-15 | 上海市农业科学院 | A kind of fumonisin B1Substrate standard substance and preparation method thereof |
| CN107319271A (en) * | 2017-08-16 | 2017-11-07 | 江门华大生物科技有限公司 | A kind of irradiation-induced degradation method of aquatic products antibiotic |
| CN108387416A (en) * | 2018-02-01 | 2018-08-10 | 辽宁出入境检验检疫局检验检疫技术中心 | Methyl mercury residue detection standard sample and preparation method thereof in shark meat |
| CN108663467A (en) * | 2018-06-21 | 2018-10-16 | 马长征 | A kind of preparation method of fish meal Analysis on amino acid components standard substance |
| 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 |
| 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 |
| CN111610073A (en) * | 2020-05-26 | 2020-09-01 | 云南省计量测试技术研究院 | Preparation method of heavy metal-containing Yunnan pseudo-ginseng standard substance |
| CN112649271A (en) * | 2020-11-18 | 2021-04-13 | 嘉兴浙华食品健康研究有限公司 | Preparation method of milk powder standard substance containing aflatoxin AFTM1 |
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