Proposal 11-12-57
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Transcript of Proposal 11-12-57
Logistics and Health Risk Assessment of Veterinary Drug and Additive in Animal Feed after ASEAN Economic Community (AEC)
Presented by Preechaya Yodrasing
ID 51216325 ENTM/M
Objective
To determine the level of residue veterinary in terms of livestock product, within ASEAN+3 and the current domestic market.
To evaluate the risk for contaminated residue of veterinary infeed of used animal.
To find out a environment that suitably for measurement the quantity of residue veterinary in terms of livestock product, and its measuring method will perform by ultrasonic-assisted extraction technique (UAE) - SPE - LC-MS/MS.
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Expected Results
To understand the overview of livestock product not only in-house and outer market but also imported product that may conceal a residue of veterinary.
To be model of management and monitoring a residue, that may cause a risk to consumer especially after the AEC was formally announce.
To know a dispersion trend of residue after the AEC was formally announce and a quantity of residue in the country.
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0
2,000,000
4,000,000
6,000,000
8,000,000
10,000,000
12,000,000
14,000,000
16,000,000
18,000,000
Feed consumption in 2004-2014(Thai Feed Mill Association, 2014)
Literature Review
Volume (Tons)
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Thailand’s total of animal feed import from ASEAN (2010-2013)(Division of Animal Feed and Veterinary Products Control, 2013)
0
50,000
100,000
150,000
200,000
2010 2011 2012 2013
0
1,000
2,000
3,000
4,000
5,000
6,000
2010 2011 2012 2013
Volume (Tons)
Value (Million Bath)
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Thailand’s total imports of animal feed from ASEAN in 2013
Raw material66.40%
Mixed material9.35%
Supplementary20.28%
Other feed3.97%
Raw material17.70%
Mixed material49.97%
Supplementary27.39%
Other feed4.93%
Ratio of quantity and animal feed imported value, segmentation by type
Countries Volume (Ton)
Value (million bath)
Vietnam 53.67 4.23
Malaysia 116.14 6.45
Singapore 4,719.02 548.82
Indonesia 6.54 2.45
China 8,603.36 939.38
Korea 1,439.68 78.91
Japan 1,520.96 143.27
Ratio of quantity imports
Ratio of value imports(Division of Animal Feed and Veterinary Products Control, 2013) Page 11
48 locals customs facilitations (Customs Facilitations, 2014)
Related Agencies of animal feed import.
1. Customs Department, Ministry of Finance.
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3. Division of Animal Feed and Veterinary Products Control, Department of Livestock Development, Ministry of Agriculture and Cooperatives.
Proceeding to evaluation, control and preserve for animal feed entrepreneur (Producer, importer and trader) follow the Feed Quality Control Act, 1982.
2. Division of Veterinary Inspector and Quarantine, Department of Livestock Development, Ministry of Agriculture andCooperatives.
Responsibly for animal quarantine, both of domestic and international, also control the movement of animal carcasses and livestock products. There are 43 outposts for in and out animal quarantine control.
Regulations The Act of Drug B.E. 2510 (1967) The Act of Feed Quality Control B.E. 2525 (1982) and revised B.E. 2542 (1999)
Related Agencies of animal feed import (Cons.)
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Import Entry
Import permit for animal feed
A license to import for animal feed into Thailand
Importer
Division of Animal Feed and Veterinary
Products Control
Imported process of animal feed is divided into two phases: pre-import and date of import.
Phases I: pre-import
Customs Facilitation
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Phases II: date of import
Inspection of the permit and other documents
Sampling for disease inspection and residue
Seizure or Withholding for further inspection
Issue the permit
Return the country of origin and legal actions
Inspect and release products
Animal Quarantine
Customs Facilitation
- DNA Ruminant- Melamine
Bureau of Quality Control of Livestock Products
The Act of Feed Quality Control
- Kasetsart University- Chulalongkorn University- Central laboratory
pass
Consideration
Not passed
Passed
by
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The outpost that mainly imported animal feed.
A=Bangkok PortB=Laem Chabang PortC=Ladkrabang Cargo ClearanceD=Suvarnabhumi Airport Cargo Clearance
AB
CD
Laos
Vietnam
Cambodia
China
Myanmar
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Antimicrobial agent used in feed
(Frank, 2010)
• Antimicrobials for the production of medicated feed is confirmed by national feed manufacturers’ associations.
13
2
Therapy
prevention
Growth promoter
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Prohibition of using chemical product in feed additive and its object Act.
Consist of
1. Avoparcin 3. Chloramphenicol 4. Carbadox5. Olaquindox 6. Nitrofurans gr.7. Nitroimidazole gr. 8. Diethylstilbestrol9. Dioxin 10. Melamine Ammeline
Ammelide Cyanuric acid
2. Beta-agonist
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The contaminated in situation that residues drug and other additives in animal feed of AEC.
In Malaysia, according from the study of Veterinarian services in 2012 found that, the amount of chicken fed up to 50% are resistant to antibiotics, Ampicillins, Sulfonamides and Tetracycline. And for an imported products, were found to be resistant to both Ampicillin, Streptomycin and other antibiotics in proportions ranging from 50 to 87% The most obviously pathogens in food such as. Listeria, Salmonella and E. coli. That is detrimental to control food quality. From the workhouses industry and manufacturing to consumers in the long term. (TheFishSite, 2014)
In China, they have been found to have used beta-agonist for a while, for example in2006, there are 336 people were taken to hospital after ate pork and its entrails(pathogens to clenbuterol) and in 2009. Police officers arrested 9 suspects who sellingpork meat those pathogens to beta-agonist. That caused more than 70 customers inGuangdong got sick. And in 2011, Chinese media have presented a farmer, in theprovince of Henan, was mixed clenbuterol into pig feed. (ASTV, 2011)
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**Contaminated assessment of residues drug in beef*** (2013) From 314 beef samples, found that there are had 128 samples contaminated
which are 40 percentage of a sampling (range of amount is 174.81 – 39,092.74 ppb)
Residue monitoring results in 2010 - 2012
Department of Livestock Development, 2013
The contaminated in situation that residues drug and other additives in animal feed of Thailand.
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The contaminated in situation that residues drug and other additives in animal feed of Thailand.
Year Type ofsample
Samplingplaces
SampleQuantity
DetectedQuantity
Type of residues
2011 Poultry feed Poultry farms 304 - -
Pig feed Pig farms 1,297 15 Tetracyclines, Sulphonamides
2012 Poultry feed Poultry farms 315 - -
Pig feed Pig farms 1,340 17 Chlortetracycline, Oxytetracycline, Tylosin A, Sulfamethazine (SMZ)
Department of Livestock Development, 2013Page 21
Literature Review
Pleadin et al. (2010) were determine the level of clenbuterol residues in muscle tissue of pigs after repeat administration in a growth-promoting dose. An anabolic dose of clenbuterol (20 μg/kg body mass per day) was administered orally to experimental group (n= 12) for 28 days. Determination of residual clenbuterol was by enzyme-linked immunosorbent assay (ELISA) as a screening method and liquid chromatography tandem mass spectrometry (LC-MS/MS) as a confirmation method. Result that the highest clenbuterol content in the muscle of treated animals was recorded on day 0 of treatment cessation (4.40± 0.37 ng/g) and significantly (p<0.05) exceeded the maximum residue limit (MRL) of 0.1 ng/g. On day 3 of withdrawal, it was 0.49±0.22 ng/g and on day 7 0.10±0.02 ng/g (at MRL); on day 14 of treatment discontinuation, clenbuterol content was below the limit of detection (<0.1 ng/g) in all samples.
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Wijayanti et al. (2011) were investigate the effect of doxycycline (a tetracycline derivative)administered at disease-prevention dose given daily in the feed and drinking water on the residue level in the broiler-chicken meat. Doxycycline at concentration of 100 ppm was mixed in the drinking water (1 g of doxycycline in 10 L of drinking water) and feed (1 g of doxycycline in 10 kg of feed). Analysis of doxycycline level was performed using high performance liquid chromatography with extraction method referring to the standard of Association of Official Analytical Chemistry. The result showed that the highest residue level was found at the first week in the group given doxycycline in drinking water (0.96±0.15 μg/g),while the highest was found at the third week in the group given doxycycline in feed (0.15±0.02 μg/g). The level of doxycycline residue exceeding the level permitted by the Indonesian National Standard (0.1 μg/g). It can be concluded that doxycycline is not recommended to be given daily both through water or feed to commercial chickens as a disease-prevention agent.
Literature Review (cons.)
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Summary of analytical methods for monitoring of Beta-agonist
Compounds Target species for
feed use
Sample treatment Analytical technique
Method performance Ref.
Extraction procedure
Clean up Detection system
Recovery (%)
Limit (ng/g)
SalbutamolRactopamineClenbuterol
Pig vortex SPE (C18 cartridges)
LC-MS 83-110 LOD:10LOQ: 50
Zhang, 2009
7 Beta-agonist Not specified
sonication SPE (polymericcartridge)
LC-MS/MS 82-110 LOD: 0.87 LOQ: 0.5-
0.92
Juan, 2010
CimaterolSalbutamol TerbutalineRactopamine
Not specified
shaking+centrifuge
SPE (MCXcartridge)
UPLC 90.1-101.4 LOD: 5-6.5LOQ: 16.7-
21.7
Qu, 2011
12 Beta-agonist Not specified
mechanicalshaking
SPE (mix-mode cartridge)
UPLC-Q/TOF MS
89.2-103.3 LOD: 1-5LOQ: 5-50
Xiu-Juan, 2013
20 prohibited veterinary drugs
Not specified
vortex+sonication
PSA sorbent LC-MS/MS 56.7-103 LOD: 0.42-5.74 LOQ 5.70-9.81
Zhang, 2013
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Summary of analytical methods for monitoring of antibiotics
Compounds Target species for
feed use
Sample treatment Analytical technique
Method performance Ref.
Extraction procedure
Clean up Detection system
Recovery (%)
Limit (ng/g)
OxytetracyclineTetracyclineChloramphenicol
Not specified
Subcritical water extraction
None LC-UV 82.1-90.0 Not reported
Wang, 2008
Multi-class CattleLambPig
shaking+sonication
PSA sorbent LC-MS/MS 51-116 LOQ:3.8-65.0
Boscher, 2010
Multi-class PigPoultry
vortex+mechanical shaking
LLE, Extraction solvent: hexane
LC-MS/MS 89.2-103.3
Not reported
Cronly, 2010
16 Sulfonamides Pig shaking+centrifuge
SPE (alumina) LC-MS/MS 80-120 LOQ: 0.5-20
Liu, 2011
ChlortetracyclineOxytetracyclineTetracyclineDoxycycline
PigPoultry
vortex+ultrasonic bath
SPE (Oasis HLB)
LC-MS/MS 80.9-119.5
LOD: 3-20LOQ: 10-50
Guo, 2012
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Methodology
Frameworks of study
Select sampling point of animal feed
Health risk assessment
Beta-agonist Antibiotics
Solid-Phase Extraction (SPE)
LC-MS/MS
Ultrasonic-assisted extraction (UAE)
Tetracyclines
TetracyclineOxytetracyclineChlortetracycline
Doxycycline
Sulfonamides
SulfadiazineSulfamethazine
SulfamethoxazoleSulfaquinoxaline
ClenbuterolSalbutamol
Ractopamine
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Analytical method
Sample preparation
-Blended and a portion of 2 g powdery feed was weighed to continue.
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Extraction(UAE)
Clean-up SPE (SCX)
LC-MS/MS
- Sample 2 g - Add Milli-Q 20 mL and 1 M HCl 2 mL
- Shaker 350 mot/min, 40 min- Ultrasonic 15 min - Centrifuge 4,000 rpm, 20 min- Filtration membrane filter, GF/B
- Precondition: MeOH 3 mL andMilli-Q 3 mL
- Wash: Milli-Q 2 mL and 2% Formic acid in water 2 mL
- Elute: 5% Ammonia in MeOH 5 mL- Dry nitrogen gas 40°C
Reconstitution: 0.1% Formic acid in water:ACN (90:10) 1 mL
Beta-agonist analysis
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Extraction(UAE) - Shaker 400 mot/min, 1 hr.
- Ultrasonic 15 min- Centrifuge 4,500 rpm, 20 min- Filtration by membrane filter, GF/B volume 10 mL And add Milli-Q 40 mL
Clean-up SPE (HLB)
LC-MS/MS
- Sample 2 g- Add MeOH:0.2M citric acid, pH3 (1:1, v/v) 30 mL
- Precondition: MeOH 2 mL and 0.04M citric acid, pH3 2 mL- Wash: 0.04M citric acid, pH3 2 mL and0.1M Sodium acetate 2 mL- Elute: MeOH 6 mL- Dry nitrogen gas 40°C
Reconstitution: MeOH +10mM Formic acid 0.5 mL
Antibiotics analysis
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Health Risk Assessment
The results obtained from this analytical
Calculated in a percentage of amount of the residue in animal products, referred from a research.x 100 = x%
y1 y2 X%
y2
y1
ba
x%
100%x a = b
bPage 32
Veterinary Drug Animal Species Tissue
Maximum Residue Limit (𝛍g/kg )
Ministry of Public Health
Department of Livestock
Development
EU CODEX Japan
Clenbutarol Not specified Edible offal - Not detected - - -
Cattle Muscle - Not detected 0.1 0.2 0.2
Liver - Not detected 0.5 0.6 0.6
Kidney - Not detected 0.5 0.6 0.6
Ractopamine hydrochloride
Cattle and Pig Muscle - - 10 10 10
Fat - - 10 10 10
Liver - - 40 40 40
Kidney - - 90 90 90
Tetracycline/Oxytetracycline/Chlortetracycline
Not specified Muscle 200 100 100 200 200
Liver 600 300 300 600 600
Kidney 1,200 600 600 1,200 1,200
Egg 400 200 200 400 400
Milk (Cattle, Sheep)
100 - 100 100 100
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MRL index
Veterinary Drug Animal Species Tissue
Maximum Residue Limit (𝛍g/kg)Ministry of Public
HealthDepartment of
Livestock Development
EU CODEX Japan
Doxycycline Pig and Poultry Muscle - 50 100 - 50Fat/Skin - 50 300 - 50
Liver - 50 300 - 50Kidney - 50 600 - 50
Other Poultry Muscle - 100 100 - 100Fat/Skin - 300 300 - 300
Liver - 300 300 - 300Kidney - 600 600 - 600
Cattle Muscle - - 100 - 100Liver - - 300 - 300
Kidney - - 600 - 600Sulfonamide Not specified Muscle 100 100 100 100 100
Fat 100 - 100 100 100Liver 100 100 100 100 100
Kidney 100 100 100 100 100Egg - 100 - - 10
Cattle, Goat and Sheep
Milk (μg/l) 25 - 100 25 10
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MRL index (cons.)
References• ASEAN Economic Community. (2013). ASEAN Economic Community History. Retrieved October 28, 2013, from Thai-AEC.com
Website: http://www.thai-aec.com/ประวตัคิวามเป็นมาประชา• ASTV. (2009). บรษิทัจนีฉาวอกี! เรยีกคนือาหารกล่องหลงัเนื้อเป้ือนสารเคม.ี Retrieved March 17, 2014, from Website:
http://www.manager.co.th/China/ViewNews.aspx?NewsID=9520000045726• ASTV. (2011). จนีเกบ็คนืผลติภณัฑเ์น้ือหม ูเหตุอือ้ฉาวปนเป้ือน “สารหมผูอม”. . Retrieved March 17, 2014, from Website:
http://www.manager.co.th/China/ViewNews.aspx?NewsID=9540000034654• Boscher, A., Guignard, C., Pellet, T., Hoffmann, L., and Bohn, T. (2010). Development of a multi-class method for the
quantification of veterinary drug residues in feedingstuffs by liquid chromatographt-tandem mass spectrometry. Journal of Chromatography A, 1217(41), 6394-6404.
• Cronly, M., Behan, P., Foley, B., Malone, E., Earley, S., Gallagher, S., Gallagher, M., Shearan, P., and Regan, L. (2010). Development and validation of a rapid multi-class method for the confirmation of fourteen prohibited medicinal additives in pig and poultry compound feed by liquid chromatography-tandem mass spectrometry. Journal of Pharmaceutical and Biomedical Analysis, 53(4), 929-938.
• Customs Facilitations. (2014). Customs Office map. Retrieved July 14, 2014, from Customs Facilitations Website: http://www.customs.go.th/wps/wcm/connect/Library+cus501th/InternetTH/About+Us/customs_area/2B75CC5BC8A4956AC217A77595536FB9
• Division of Animal Feed and Veterinary Products Control. (2013). Comparison data between quantity and imported values of animal feed in 2012-2013. Retrieved March 18, 2014, from Division of Animal Feed and Veterinary Products Control Website: http://afvc.dld.go.th/forum.php?mod=viewthread&tid=161&extra=Array
• Division of Animal Feed and Veterinary Products Control. (2014). History of Division of Animal Feed and Veterinary Products Control. Retrieved March 18, 2014, from Division of Animal Feed and Veterinary Products Control Website: http://afvc.dld.go.th/forum.php?mod=viewthread&tid=74&extra=page%3D1
• Division of Veterinary Inspector and Quarantine. (2014). History of Division of Veterinary Inspector and Quarantine. Retrieved December 2, 2014, from Division of Veterinary Inspector and Quarantine Website: http://aqi.dld.go.th/th/index.php?option=com_content&view=article&id=174&Itemid=57
• Frank, A. (2010). Evaluation of the EU legislative framework in the field of medicated feed. Retrieved February 20, 2014, from Food Chain Evaluation Consortium (FCEC) Website: http://ec.europa.eu/food/food/animalnutrition/labelling/medicated_feed_report_20100224.pdf Page 35
• Guo, L., Chen, Y., Zhang, L., Yang, W., and He, P. (2012). Development and validation of a liquid chromatographic tandem mass spectrometric method for determination of chlortetracycline, oxytetracycline, tetracycline, and doxycycline in animal feeds. Journal of AOAC International, 95(4), 1010-1015.
• Juan, C., Igualada, C., Moragues, F., Leon, N., and Manes, J. (2010). Development and validation of a liquid chromatography tandem mass spectrometry method for the analysis of beta-agonists in animal feed and drinking water. Journal of Chromatography A, 1217(39), 6061-6068.
• Liu, R., He, P., Li, Z., and Li, R. (2011). Simultaneous determination of 16 sulfonamides in animal feeds by UHPLC-MS-MS. Journal of Chromatographic Science, 49(8), 640-646.
• Pleadin, J., Vulic, A., Persi, N., and Vahcic, N. (2010). Clenbuterol residues in pig muscle after repeat administration in a growth-promoting dose. Journal of Meat Science, 86(3), 733-737.
• Qu, C. H., Li, X. L., Zhang, L., Xi, C. X., Wang, G. M., Li, N. B., and Luo, H. Q. (2011). Simultaneous determination of cimaterol, salbutamol, terbutaline and ractopamine in feed by SPE coupled to UPLC. Journal of Chromatographia, 73(3-4), 243-249.
• Thai Feed Mill Association. (2014). Animal population and Feed Consumption. Retrieved February 20, 2014, from Thai Feed Mill Association Website: http://www.thaifeedmill.com/tabid/56/Default.aspx
• TheFishSite. (2014). Malaysian Consumers urge ban of antibiotics in animal feed. Retrieved March 16, 2014, from National Bureau of Agricultural Commodity and Food Standards Website: http://www.acfs.go.th/read_news.php?id=11863&ntype=07
• Wang, L., Yang, H., Zhang, C., Mo, Y., and Lu, X. (2008). Determination of oxytetracycline, tetracycline and chloramphenicol antibiotics in animal feeds using subcritical water extraction and high performance liquid chromatography. Journal of Analytica Chimica Acta, 619(1), 54-58.
• Wijayanti, A. D., Wihandoyo., and Rosetyadewi, A. W. (2011). The comparison of Doxycycline residue in meat of broiler chickens administered in feed and water. Journal of Animal Science and Technology, 34(3), 175-178.
• Xiu-Juan, W., Feng, Z., Fei, D., Wei-Qing, L., Qing-Yu, C., Xiao-Gang, C., and Cheng-Bao, X. (2013). Simultaneous determination of 12 beta-agonists in feeds by ultra-high-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry. Journal of Chromatography A, 1278, 82-88.
• Zhang, G. J., Fang, B. H., Liu, Y. H., Wang, X. F., Xu, L. X., and Zhang, Y. P. (2013). Development of a multi-residue method for fast screening and confirmation of 20 prohibited veterinary drugs in feedstuffs by liquid chromatography tandem mass spectrometry. Journal of Chromatography B, 936, 10-17.
• Zhang, L. Y., Chang, B. Y., Dong, T., He, P. L., Yang, W. J., and Wang, Z. Y. (2009). Simultaneous determination of salbutamol, ractopamine, and clenbuterol in animal feeds by SPE and LC-MS. Journal of Chromatographic Science, 47(4), 324-328.
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