CN106404493A - Standard streptomycin samples of chicken, preparation method and application - Google Patents
Standard streptomycin samples of chicken, preparation method and application Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
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Abstract
The invention provides standard streptomycin samples of chicken, a preparation method and an application and belongs to the technical field of analytical chemistry. Chickens are fed with feed containing streptomycin, so that in-vivo tissue of live chickens contains the streptomycin, the chickens are killed after drug application, feathers and skin are removed, the chicken is taken and homogenized, minced meat is prepared and subjected to vacuum freeze drying, sieving, bottling and packaging, and standard samples of lyophilized chicken powder containing the streptomycin are obtained. The method solves the problem that treatment results such as extraction, purification and the like are more different from routine analysis samples due to the fact that the a target and matrix combining condition is incompletely consistent with a real detection sample, and the standard samples are material standard samples, are homogenous, stable, free of preservatives and antioxidants and easy to store and are used for proficiency testing of a streptomycin drug residue testing project, verification of a detection method, calibration of testing equipment as well as quality control and assessment of testing results.
Description
Technical field
The invention belongs to analytical chemistry field, it is related to a kind of preparation of the natural basal body standard sample of residue of veterinary drug, specifically
Ground is said, is related to a kind of chicken streptomycin residual matrix freeze-dried powder standard sample and preparation method and application.
Background technology
Streptomysin (streptomycin) is the antibiotic extracting from the nutrient solution of grey streptomycete in nineteen forty-four, molecular formula
For C21H39N7O12, molecular weight is 581, white powder, water-soluble more stable to heat under pH value 3 to 7, have hydrochloride and
The products such as sulfate.Streptomyces, in Aminoglycoside alkali compounds, is a kind of organic base of antibiosis, can be reasonably resistant to many
Bacterium, it is combined with tubercle bacillus thalline RNP body protein, serves interference tubercle bacillus protein synthesis
Effect, thus kill or suppression growth of bacillus tubercle effect, its as feed addictive and therapeutic agent agricultural, animal husbandry and
Extensively apply in aquaculture.Streptomysin has certain toxic and side effect to human body.Dihydrostreptomycin (dihydrostreptomycin)
It is the derivative of streptomysin, after the aldehyde radical of strepto- sugar moieties is reduced into primary alconol base in streptomysin molecule, just become double hydrogen strepto-s
Element, molecular formula is C21H41N7O12, molecular weight is 583.44.Its antibacterial efficacy is roughly the same with streptomysin, but to auditory nerve
Toxicity is bigger than streptomysin, and streptomysin and dihydrostreptomycin are all important medicines in aminoglycosides antibiotics.In aquatic products and poultry
Herd in cultivation, the two is often used guard against various animality diseases or is added to promotion animal growth in feed.Food
In if remaining excessive streptomysin or dihydrostreptomycin, serious harm can be caused to people, such as infringement vestibular nerve and ear
Cochlear nerve, leads to dizziness and dysacousis, streptomysin and dihydrostreptomycin also to have potential teratogenesis.
European Union's clear stipulaties prohibit the use of such medicine as the growth-promoting additive of domestic animal；U.S. FDA is secondary due to its poison
Effect and easily generation drug resistance, also extremely pay close attention to the residual of such medicine in animal derived food.2377/90/EEC
(703/2007 revision) regulation animal food muscle, fat, liver streptomycin MRL MRL are 500 μ g/kg,
It is 1000 μ g/kg in kidney, be 200 μ g/kg in breast.Strepto- in Codex Committee on Food (CAC) regulation animal food muscle
The MRLs of element is 0.5mg/kg, and the MRLs in liver is 0.5mg/kg, and the MRLs in kidney is 1.0mg/kg.China is animal derived
Food residue material Supervisory Surveillance Program streptomycin and dihydrostreptomycin are banning drugs, require method detection limit in eel matrix
(being counted with streptomysin and dihydrostreptomycin total amount) is 10 μ g/kg.
In food safety detection system, standard sample plays central role to whole detection quality control system.In state
On border, a kind of foundation of analysis method of Residual Veterinary Medicines needs the sample test through 3 types：Controlled tissue or liquid, use
Medicine is enhanced to or the sample close to maximum allowable level (MRL) and the tissue sample itself with medicament residue, thus ensureing
Analysis method can have certain sample substrate scope of application and repeatability.European Union is to wild animal resources method and results expression
Regulation (2002/657/EC) in explicitly pointed out and needed to carry out detection process control using material standard sample it is seen that material object
Tool in detection of veterinary drugs in food for the standard sample is of great significance.
Currently used for the mainly pure standard items of streptomycins residue detection, detection quality control mainly pass through to
Tested and analyzed after adding pure standard items in sample, it is real in vivo that this analysis method cannot represent target analytes
Exist state it is impossible to truly reappear medicine after natural metabolism extraction efficiency in animal body it is impossible to reflection method
Accuracy.Because object and matrix are not quite identical and lead to extract, purify etc. with reference to situation and true detection sample
There is larger difference with routine analysis sample, thus affecting reliability and the validity of result in reason result.In addition, general standard sample
Be added with the antioxidants such as vitamin C in product early stage preparation process, lead to standard sample the later stage related drugs residue detection
In the application process of analysis etc., experimental result is interfered and affect.
Content of the invention
Medicine can not truly be reappeared to solve the detection of prior art streptomycin class medicament residue through natural metabolism
Extraction efficiency in animal body, it is impossible to the accuracy of reflection method, affects reliability and the validity of result afterwards, and exists anti-
Oxidative attack uses the technical problem of result, it is an object of the present invention to provide the preparation of chicken streptomycin standard sample
Method and application.It is a further object to provide the chicken streptomycin standard sample of this method preparation.
The present invention be employed technical scheme comprise that by solving above-mentioned technical problem：The preparation of chicken streptomycin standard sample
Method is it is characterised in that comprise the following steps：
A live chickens), are selected, artificial feeding is contained the feed of streptomysin, made to contain streptomysin in chicken body；
B after), administration terminates, slaughter, take chicken muscle, blend, mix and make meat gruel, homogeneous, vacuum freeze drying obtain slightly
Sample；
C), study described in grinding steps B, sieves, and obtains chicken freeze-dried powder standard sample；
D), encapsulate described standard sample, stored refrigerated；
E uniformity and the stability of described standard sample), are checked；
F), definite value is carried out to the content of streptomycin that has in described standard sample.
The selection of animal used as test in described step A, operates and is：Screen in chicken farm that individual health, size be homogeneous, counterpoise
The chicken of 1.5-2.5kg, male and female are random, isolate, feeding 1 time during the daily morning 8, treat after raising and train 3 under 20 DEG C of -25 DEG C of environment
With.
In described step A, medicine adds, and operates and is：Weigh 0.2～2.4g streptomysin, be added in 2.0kg feed, stirring
Uniformly, that is, make the feed A that streptomysin concentration is 0.1～1.2g/kg.
Tested using artificial feeding in described step A, operate and be：The daily feeding feed stuff A 50g of every chicken, that is, offer medicine
Dosage is 2～40mg/kg body weight；By daily single, successive administration 3-5 day.
Time of slaughtering in described step B is 3～5h after last administration terminates.
Vacuum freeze drying condition in described step B is：The precooling stage：- 80 DEG C -- 30 DEG C, corresponding pre-coo time
0.5-10h；The vacuum refrigeration stage：Stress control in 0.01-1.0mbar, corresponding time 8-15h；The drying sublimation stage：-10℃-
30 DEG C, corresponding time 2-10h.
The mesh number that described step C is sieved is 30～80 mesh.
In described step D, bottle used is the white polyethylene plastic bottle with aluminium-foil gasket, often bottled 10g freeze-dried powder,
Electromagnetic induction covers, and 2-8 DEG C stored refrigerated.
The content of streptomycin of described standard sample is 100 μ g/kg～2000 μ g/kg
The remarkable advantage of the present invention is：
1) feed the feed containing streptomysin to chicken, select opportune moment, slaughter, take muscle parts homogenate to make meat gruel,
Freeze-drying, sieves, and sealed packaging is packed；
2) uniformity testing, stability study and cooperation setting examination, can by being administered control and the selection on collection opportunity
Obtain the object bonding state of expected content containing the streptomysin matrix positive material consistent with actually detected sample；
3) product of the present invention can transport at normal temperatures, long shelf-life, and object and matrix are combined situation and examined with true
Test sample product are consistent, and standard sample is material standard sample, uniform and stable, preservative free and antioxidant, easily preserve, for strepto-
The proficiency testing of plain class medicament residue test event, the checking of detection method, the calibration of tester, the quality control of test result
System and examination.
Brief description
Fig. 1 is the chemical structural formula of streptomysin.
Fig. 2 is the standard sample preparation technology flow chart of the present invention.
Fig. 3 is the LC-MS spectrogram of the standard sample of the present invention.
Specific embodiment
As shown in Fig. 2 the preparation method of the chicken streptomycin standard sample of the present invention, comprise the following steps：A) medicine
Feed；B) sampling, decontamination, homogenate；C) vacuum freeze drying；D) grinding, screening, sample mixing, encapsulation；E) uniformity and stability
Inspection；F) determine content of streptomycin.
With reference to specific embodiment, the present invention will be further described.It should be understood that following examples are merely to illustrate this
Invention is not for restriction the scope of the present invention.The experimental technique of unreceipted actual conditions in the following example, generally according to normal
Rule condition, or according to the condition proposed by manufacturer.
Embodiment 1
A kind of preparation method of chicken streptomycin standard sample, it comprises the following steps that：
(1) selection of animal used as test：Screen individual health, homogeneous, counterpoise 2kg the carnivorous white feather chicken of size in chicken farm,
Male and female are random.Under 25 DEG C of environment isolate, feeding 1 time during the daily morning 8, after raising and train 3, therefrom select 18 stand-by；
Medicine is raised：Weigh 1.6g streptomysin, be added in 2.0kg feed, after stirring, after feeding 18 is only raised and train
Chicken, every chicken daily feeds 50g feed, feeding 1 time during the daily morning 8.Dosage is 20mg/kg body weight, continuously dispensing 3
Day；
(2), after being administered 3, after that is, last administration terminates 3h, take chicken muscle after slaughtering, blend, mix and make meat gruel；
(3) vacuum freeze drying：Freeze-drying is carried out using vacuum freeze drier (CHRiST Epsilon 2-6D),
Material thickness 2cm, -50 DEG C of precooling 6h, 0.1mbar vacuum refrigeration 10h, -10 DEG C -30 DEG C are rapidly heated 8h are dried, until complete
White drying, obtains the positive lyophilized meal of streptomysin；
(4) grind, sieve：Freeze-dried powder is pulverized with medicinal herb grinder, tissue grinder fine grinding, crosses 30 mesh sieves, takes lower part of screen
Point；
(5) dispense and preserve：With the white polyethylene plastic bottle packing with aluminium-foil gasket, often bottled 10g freeze-dried powder, electricity
Magnetic induction covers, and 2 DEG C stored refrigerated.
Detect the sample of embodiment 1 preparation using LC-MS, result is as shown in Figure 3 it was demonstrated that contain strepto- in standard sample
Element.
Embodiment 2
Repeat the preparation process in embodiment 1, different experiment conditions is in the present embodiment：
1) animal used as test selects body weight is 1.5kg；
2) weigh streptomysin 0.2g；
3) three kinds of administration of medication dosage are 3.3mg/kg body weight；
4) successive administration 5 days；
5) last administration is slaughtered after terminating 3h；
6) -80 DEG C of precooling 0.5h, 0.01mbar vacuum refrigeration 8h, is rapidly heated and 2h is dried；
7) 50 mesh sieves are crossed；
8) 5 DEG C stored refrigerated.
Embodiment 3
Repeat the preparation process in embodiment 1, different experiment conditions is in the present embodiment：
1) animal used as test selects body weight is 2.5kg；
2) weigh streptomysin 2.4g；
3) three kinds of administration of medication dosage are 24mg/kg body weight；
4) successive administration 4 days；
5) last administration is slaughtered after terminating 4h；
6) -30 DEG C of precooling 10h, 1.0mbar vacuum refrigeration 15h, is rapidly heated and 10h is dried；
7) 80 mesh sieves are crossed；
8) 8 DEG C stored refrigerated.
Embodiment 4
Uniformity and stability test are carried out to sample in embodiment 1：
1. uniformity testing
Uniformity testing is carried out using one-way analysis of variance method, randomly draws the sample of 12 bottles of examples 1 preparation, every bottle
Sample parallel determination 2 times.All test portions are tested under the conditions of repeatability with random order, that is, by identical in same laboratory
Librarian use identical method of testing and instrument are tested within a short period of time.
Method of testing：Weigh 0.5g sample, plus 4.5ml water reduction 15min, by GB/T 21323-2007 animal tissue
Mensure High Performance Liquid Chromatography/Mass Spectrometry/the mass spectrography of aminoglycoside medicaments residual quantity is detected.
Evaluation for Uniformity is carried out using following one-way analysis of variance.
Extract i sample (i=1,2,3 ... m), each sample test under repeat condition j time (j=1,2,3 ... n).
The testing mean of each sample
The overall average of whole samples test
Test total degree
Sample room quadratic sumAll square
Quadratic sum in sampleAll square
Free degree f1=m-1
f2=N-m
Statistic
Uniformity testing result and evaluation are shown in Table 1.
The sample homogeneity testing result of table 1 example 1 preparation and statistical analysis
Unit：μg/kg
Result above understands：As α=0.05, f1=11, f2=12, look into F distribution table, F critical value is 2.72, because of F statistical value
(1.90)<F critical value 2.72, show in sample and sample room there was no significant difference, illustrate that sample is uniform, disclosure satisfy that matter
The requirement of experiment such as control.
Using same procedure, verify the uniformity of the standard sample that embodiment 2,3 is obtained, F is more equal than respectively 2.05,2.20
Less than F critical value 2.72, show in the standard sample sample that embodiment 2,3 is obtained and sample room there was no significant difference, sample is described
Product are uniform, disclosure satisfy that the requirement of experiment such as Quality Control.
2. stability test
2.1 long-time stability inspections
According to the rear sampling principle dredged close before time interval, randomly draw for stability test by the following time respectively
The sample of packaged embodiment 1 preparation：0th, 2,4,6,9,12,18 months.Extract 3 samples every time to be tested.Whole
In stability test, personnel used, instrument, method of testing are all identical with uniformity test with laboratory.Result and statistical analysis
As shown in table 2.
With the stability of linear fit model evaluation standard sample, the time is represented with X, Y represents target medicine in standard sample
The content of thing, slope b1Calculated with following formula：
The estimate of slope：
The estimate of intercept：
The standard deviation publicity of every on straight line：
The uncertainty related to slope：
When | b1| ＜ t0.95,n-2·s(b1), show that slope variation is not notable, that is, standard sample is stable.
Table 2 sample long-time stability check and statistical analysis
Unit：μg/kg
The free degree is the distribution of n-2 and p=0.95 (95% confidence level) is t0.95,(n-2)=2.57, due to | b1| ＜
t0.95,n-2·s(b1), therefore slope is inapparent, that is, do not observe unstability, verifies the steady of the standard sample that embodiment 1 is obtained
Qualitative good.
2.2 short-term stability inspections
Short-term stability is checked：Investigate stability under traffic condition for the standard sample, mark is transported using express delivery mode
Quasi- sample, most area 3-4 days can receive sample, and extremely individual otherwise also can be sent within 9 days.During transport, by sample
It is positioned in heat insulation cellular plastics case and then puts ice cube and transport together.During transport, then sample is positioned in heat barrier foam case
Put ice cube to transport together.Randomly draw 6 bottles of cryopreserved sample, send it to Xinjiang Urumqi with Express Mail Service mid-August,
Untouched after reaching Urumchi return Dalian again, the same manner randomly draws 6 bottles of cryopreserved sample, with Express Mail Service in 12
The middle of the month sends it to Heilungkiang Mo River, untouched after reaching Mo River returns Dalian again.Sample is sent and is returned all times for 10d.Right
The sample (sample after transport) returned is detected using GB/T 21323-2007 method, and (transports with the sample without transport
Front sample) compare analysis experiment.
With t method of inspection, the measured value of sample before and after transport is carried out with consistency check, inspection formula is：
Statistic t calculates：
Calculate t experiment, withRelatively, if t experiment less than critical value then it is assumed that the spy of this standard sample
Property value do not occur conspicuousness change, otherwise it is assumed that there being significant difference.The results are shown in Table 3.
Table 3 sample short-term stability assay and statistical analysis
As can be drawn from Table 3, t experiment value is respectively less thanValue of tabling look-up (2.228), shows the spy of this standard sample
Property value transport before and after measured value there is uniformity.The short-term stability of the standard sample that checking embodiment 1 is obtained is good.
Using above-mentioned same procedure, verify the stability of the standard sample that embodiment 2,3 is obtained, slope is not all notable, not
Observe the standard sample unstability that embodiment 2,3 is obtained, result shows that the standard sample stability that embodiment 2,3 is obtained is good
Good.
Embodiment 5
The definite value of standard sample streptomycin content：
Eight laboratories carry out collaborative definite value using the standard sample that LC-MS/MS method is prepared to embodiment 1.To process
Uniformity and the qualified sample of stability test, randomly draw 40 bottles, and the laboratories being distributed to 8 participation definite values respectively are examined
Survey, the results are shown in Table 4.The value data in 8 laboratories investigates it using Xia Piluo-Weir gram (Shapiro-Wilk) method of inspection
Normality.On the premise of approximately meeting normality, then it is different to check each laboratory data of confirmation whether there is through Grubb ' s method
Constant value, checks each laboratory value data whether equally accurate with Cochran (Cochran), and result shows that all of data is all passed through
Inspection, each laboratory measuring accuracy is consistent.
Table 4 cooperation definite value laboratory test results
Unit：μg/kg
Definite value result by standard value and does not know to form.For Duo Jia laboratory cooperation definite value mode, standard value is many families
The overall average in laboratory.Standard value always do not know be mainly derived from the uncertainty of definite value result, sample inhomogeneities is drawn
The uncertainty that rises, the uncertainty that causes of stability.
It is assumed that each variable is independent, the uncertainty relevant with CRM characteristic value is represented by：
Wherein ucharIt is the uncertainty that designated value process introduces, ubbRefer to the uncertainty that sample inhomogeneities introduces,
ultsRefer to the uncertain of sample long-time stability introducing, ustsRefer to the uncertainty that sample short-term stability introduces.
Extension is uncertain can be multiplied by Coverage factor by combined standard uncertainty, take k=2 (confidential interval 95%), obtain expansion
Exhibition is uncertain：U=k × uCRM
By statistical analysis, by the way of standard value ± expanded uncertainty, represent definite value result, final determination is implemented
The standard sample of preparation in example 1：Content of streptomycin (630 ± 33) μ g/kg, k=2.
Using above-mentioned same procedure, definite value that the content of streptomycin of the standard sample of embodiment 2,3 is cooperated, using mark
The mode of quasi- value ± expanded uncertainty represents, respectively (104 ± 6) μ g/kg, k=2, (810 ± 45) μ g/kg, k=2.
Embodiment 6
The application of chicken streptomycin standard sample：
First streptomysin standard sample prepared by embodiment 1 is distributed to corresponding laboratory 1-3 and its personnel, standard is provided
Operating Guideline, is then tested, and reports testing result (μ g/kg represents) and uncertainty of measurement, with En value to each experiment knot
Fruit is evaluated, and En number is calculated by following formula：
In formula,
LAB and REF represents the test result in participate in the experiment laboratory and standard sample respectively；
ULABAnd UREFYour laboratory and the uncertainty of measurement of standard sample test result represented respectively.
Criterion：| En |≤1, satisfactory result；When the absolute value of En number is more than 1, for being unsatisfied with result, laboratory should be adjusted
Look into reason, take further corrective action and re-start.
As shown in table 5, laboratory 2 and 3 | En | are respectively less than 1, are satisfactory result, illustrate that laboratory 2 and 3 possesses corresponding inspection
Survey ability, | the En | in laboratory 1, more than 1, for result that is dissatisfied or peeling off, illustrates that laboratory 1 does not possess corresponding detection energy
Power.For the laboratory reporting dissatisfied or the result that peels off, reason should be searched, propose corresponding measures to rectify and reform, improve detection water
Flat.The standard sample of result display preparation has reached test requirements document, can effectively ensure that Determination of Streptomycin Residues detection Intercomprison
Test quality control activity.
Table 5 sample is used for quality control action result
The standard sample of the preparation method preparation using the present invention can also be used for the checking of detection method, survey further
The calibration of test instrument, quality examination of test result etc..
Above-mentioned embodiment is only used for explaining the present invention, rather than limits the invention, the present invention spirit and
In claims, any modifications and changes that the present invention is made, both fall within protection scope of the present invention.
Claims (9)
1. the preparation method of chicken streptomycin standard sample is it is characterised in that comprise the following steps：
A live chickens), are selected, artificial feeding is contained the feed of streptomysin, made to contain streptomysin in chicken body；
B after), administration terminates, slaughter, take chicken muscle, blend, mix and make meat gruel, homogeneous, vacuum freeze drying obtain study；
C), study described in grinding steps B, sieves, and obtains chicken freeze-dried powder standard sample；
D), encapsulate described standard sample, stored refrigerated；
E uniformity and the stability of described standard sample), are checked；
F), definite value is carried out to the content of streptomycin that has in described standard sample.
2. the preparation method of chicken streptomycin standard sample as claimed in claim 1 is it is characterised in that in described step A
The selection of animal used as test, operates and is：Chicken farm screen individual health, homogeneous, counterpoise 1.5-2.5 kg the chicken of size, male and female with
Machine, isolates, feeding 1 time during the daily morning 8 under 20 DEG C of -25 DEG C of environment, stand-by after raising and train 3.
3. the preparation method of chicken streptomycin standard sample as claimed in claim 1 is it is characterised in that in described step A
Medicine adds, and operates and is：Weigh 0.2 ~ 2.4 g streptomysin, be added in 2.0 kg feeds, stir, that is, make strepto-
Plain concentration is the feed A of 0.1 ~ 1.2 g/kg.
4. the preparation method of chicken streptomycin standard sample as claimed in claim 1 is it is characterised in that in described step A
Tested using artificial feeding, operate and be：Every chicken daily feeding feed stuff A 50 g, that is, dosage is 2 ~ 40mg/kg body
Weight；By daily single, successive administration 3-5 day.
5. the preparation method of chicken streptomycin standard sample as claimed in claim 1 is it is characterised in that in described step B
Time of slaughtering be 3 ~ 5 h after last administration terminates.
6. the preparation method of chicken streptomycin standard sample as claimed in claim 1 is it is characterised in that in described step B
Vacuum freeze drying condition be：The precooling stage：- 80 DEG C -- 30 DEG C, corresponding pre-coo time 0.5-10 h；Vacuum refrigeration
Stage：Stress control is in 0.01-1.0 mbar, corresponding time 8-15h；The drying sublimation stage：- 10 DEG C -30 DEG C, when corresponding
Between 2-10 h.
7. the preparation method of chicken streptomycin standard sample as claimed in claim 1 is it is characterised in that described step C mistake
The mesh number of sieve is 30 ~ 80 mesh.
8. the preparation method of chicken streptomycin standard sample as claimed in claim 1 is it is characterised in that in described step D
Bottle used is the white polyethylene plastic bottle with aluminium-foil gasket, often bottled 10g freeze-dried powder, and electromagnetic induction covers, and 2-8 DEG C cold
Hide and preserve.
9. the standard sample of the preparation method preparation of the chicken streptomycin standard sample according to any one of claim 1 ~ 8
Product are it is characterised in that the content of streptomycin of described standard sample is 100 μ g/kg ~ 2000 μ g/kg.
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| CN111579320A (en) * | 2020-04-26 | 2020-08-25 | 西安文理学院 | Egg standard substance containing chloramphenicol, preparation method and application |
| CN113514293A (en) * | 2021-04-16 | 2021-10-19 | 四川省食品药品检验检测院 | Preparation method and application of recessive malachite green standard sample in snakehead meat powder |
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