Extraction and Cleanup Protocols for LC-MS/MS Multiresidue Determination of Veterinary Drugs in Tissue and Milk Samples
|
|
- Leon Andrews
- 5 years ago
- Views:
Transcription
1 Extraction and Cleanup Protocols for LC-MS/MS Multiresidue Determination of Veterinary Drugs in Tissue and Milk Samples Malin Wangler, Waters Sweden Michael S. Young and Kim vantran Waters Milford 2011 Waters Corporation 1
2 Overview There is a need for multiresidue UPLC-MS methods that can identify and quantify a wide range of veterinary drug residues from many drug classes Solvent extraction (acetonitrile or methanol) can be effective for many of these compounds in meat and milk Polar, highly water soluble drugs such as salbutamol are not well recovered using this approach Aqueous buffer extraction can also be effective for many compounds Fat soluble compounds such as dexamethasone are not well recovered using this approach Traditional SPE enrichment and cleanup (retention/wash/elution) has limited utility for multi-residue analysis; the range of polarity/solubility among the compounds is very challenging Dispersive or pass-thru SPE is preferred for multi-residue methods Traditional SPE is still a powerful procedure and is preferred for isolation/cleanup of individual compounds or compound classes 2011 Waters Corporation 2
3 Optimized Method for Tetracyclines Example of Class Specific Method Oasis MAX SPE protocol Condition/Equilibrate 2 ml MeOH, 2 ml water Load Sample from pretreatment Wash ml 5% NH 4 OH/water Wash ml methanol Elute : 0.5 ml 45:55 acetonitrile/75mm oxalic acid Pretreatment Mix 1.5 ml milk with 6 ml ph 4 McIivaine buffer Centrifuge Take supernatant/adjust to ph 10 with 0.75 ml 1 M NaOH assures analytes are anions removes neutrals or bases neutralizes compounds to release from sorbent (oxalic acid stabilizer) - Recovery % at the 100 ng/g level - Virtually no suppression/enhancement Method great for tetracyclines but not suitable for multi-class analysis 2011 Waters Corporation 3
4 Goals/Observations The purpose of this ongoing study is to evaluate simple sample preparation strategies (extraction/cleanup) for multiresidue analysis of veterinary drugs in meat and milk. No internal standards are used: recovery is not corrected for by comparison with internal standards the observed precision is typical for external standard calibration. Many compounds show significant ion-suppression. This may not be a serious impediment to useful analytical performance if matrix matched standards are employed and the response of the compound is sufficient. Among the goals of future work will be advances in SPE cleanup to reduce matrix effects Waters Corporation 4
5 Veterinary Drug Classes in This Study Tetracycline Fluoroquinolone Sulfonamide Macrolide tetracycline enrofloxacin sulfamethazine erythromycin Beta Lactam NSAID Steroid Beta-adrenergic salbutamol oxacillin phenylbutazone dexamethasone 2011 Waters Corporation 5
6 Instrumentation for This Study Xevo TQ ACQUITY UPLC ACQUITY TQD Used for meat analysis Used for milk analysis 2011 Waters Corporation 6
7 Veterinary Drugs ACQUITY UPLC Conditions Column: ACQUITY CSH C18 1.7µm 100 x 2.1 mm Mobile phase A: 0.1% formic in water B: 0.1% formic acid acetonitrile Time (min) Gradient Table Flow % A (ml/min) % B Curve Injection volume: 7 µl Injection mode: partial loop injection Sample diluent: 20:80 ACN:water Column temperature 30 C Weak Needle Wash: 10:90 acetonitrile:water (600 μl) Strong Needle Wash: 50:30:40 water:acetonitrile:ipa (200 μl) Seal wash: 10:90 acetonitrile: water Initial Initial Waters Corporation 7
8 MS Conditions Principal MRM Transitions Polarity ES+ (Except Chloramphenicol ES-) Capillary (kv) 2.80 Extractor (V) 3.00 Source Temperature ( C) 150 Cone Gas Flow (L/Hr) 30 Desolvation Temperature ( C) 500 Desolvation Gas Flow (L/Hr) 1000 Collision Gas Flow (ml/min 0.15 MassLynx V4. Waters Xevo TQ MS: meat analysis conditions shown Waters ACQUITY TQD : milk analysis similar MS conditions and same transitions Compound Principal MRM Cone CID Amoxicillin 366> Carbadox 263> Ciprofloxacin 332> Chloramphenicol 321> Chlortetracyline 479> Dexamethasone 393> Enrofloxacin 360> Erythromycin 734> Lincomycin 407> Oxacillin 402> Oxytetracycline 461> Penicillin-G 335> Phenylbutazone 309> Ractopamine 302> Salbutamol 240> Sulfamerazine 265> Sulfamethazine 279> Sulfanilamide 173> Tetracycline 445> Tylosin 916> Waters Corporation 8
9 LC/MS Functions Function 1 Sulfanilamide Salbutamol Ractopamine Lincomycine Function 2 Carbadox Sulfamerazine Sufamethazine Erthromycin Tylosin Function 3 Phenylbutazone Penicillin Dexamethasone Oxacillin Function 4 Ciprofloxacin Enrofloxacin Function 5 Tetracyline Oxytetracycline Chlortetracyline Function 6 Chloramphenicol Dwell time sec. Two transitions per analyte Minimum of 10 datapoints across each chromatographic peak 2011 Waters Corporation 9
10 % % Typical LC/MS/MS Response Erythromycin (10 ng/g meat sample) Comparison of response for principal (top) and confirmatory transitions for erythromycin (Waters Xevo TQ) VET02FA060711_ S/N:RMS= : MRM of 10 Channels ES > (Erthromycin) 4.85e VET02FA060711_87 S/N:RMS= : MRM of 10 Channels ES > (Erthromycin) 4.55e Time 2011 Waters Corporation 10
11 Analytical Options Sample Preparation Strategies Perform both aqueous and acetonitrile extraction on the same tissue or milk sample Tedious and time consuming multi-step extraction o strategy results in two extracts requiring separate workup before combining for one LC/MS analysis o provides best recovery of the widest range of compounds Perform extraction using a mixed acetonitrile/aqueous system Less steps required for analysis o strategy results in one rather messy extract that requires workup o workup is straightforward o reasonable recovery and cleanup is possible for a wide range of compounds 2011 Waters Corporation 11
12 Definitions Ion-suppresion or enhancement (Matrix effect) - A decrease (suppression) or increase (enhancement) in the MS response for an analyte caused by the presence of interfering substances resulting from the sample matrix. - The matrix effect is calculated by comparison of analyte response for a standard prepared in sample matrix with analyte response for a standard prepared in pure solvent. Recovery - The amount of an analyte recovered by the analytical method. - Recovery of an analyte from a sample is calculated by comparison of the response shown for an analyte fortified into the sample matrix prior to all sample preparation with response shown for a blank matrix sample fortified with the analyte after all sample preparation steps Waters Corporation 12
13 Part 1 Milk Analysis 2011 Waters Corporation 13
14 Milk Composition Typical Cow s Milk Approximately 14 % solids o 4 % fat o 4 % protein o 5 % sugar (lactose) o 85 % water 2011 Waters Corporation 14
15 Veterinary Residues in Milk Multiresidue LC/MS Analysis Typical Sample Preparation Strategies Precipitation/extraction with strong buffer (McIlvaine ph 4) followed by SPE o good for tetracyclines, beta-adrenergics, polar sulfonamides, fair for fluoroquinolones, o poor recovery of most other compounds Precipitation/extraction with 3:1 acidic acetonitrile with SPE cleanup o excellent protein precipitation o poor recovery of tetracyclines, beta-adrenergics, polar sulfonamides o good recovery of most other compounds This study: two-step precipitation/extraction o good recovery of a wide range of compounds 2011 Waters Corporation 15
16 Typical Recoveries From Milk Comparison of Precipitation/Extraction Techniques Drug Class 3:1 ACN Aq Buffer 1:1 ACN* Beta-adrenergic <10 ~100 >80 Tetracycline <25 >70 >25 Fluoroquinolone >50 >50 >50 Macrolide >60 <35 >60 Beta-Lactam >70 <30 >70 Steroid >70 <10 >70 *Conclusion: -Procedure chosen for this study -Extraction/precipitation of milk with an equal volume of acetonitrile provides recovery of the widest range of compounds However - insufficient protein precipitation See also: Stolker et. al., Anal. Bioanal. Chem. 391, 2309 (2008) 2011 Waters Corporation 16
17 Analytical Method For This Study Milk 2 ml Sample Initial Extraction/Precipitation Pipet 2 ml sample into centrifuge tube Add 2 ml acetonitrile 8000 x g Take 2 ml supernatant provides good recovery of most compounds minimal extraction of fat much protein in extract Protein Precipitation Add 3 ml acetonitrile(0.2% formic acid) 8000 x g Take 1 ml supernatant secondary protein precipitation step removes most residual protein without significant loss of polar analytes SPE Cleanup Sep-Pak C18 (1 cc, 100 mg) Evaporate and reconstitute 2011 Waters Corporation 17
18 SPE Cleanup Sep-Pak C18 (pass-thru mode) Condition 1 ml 80:20 acetonitrile/water Pass-Thru/Collect 1 ml protein ppt sample install collection tubes 1 cc 100 mg Rinse/Collect 0.5 ml 80:20 acetonitrile/water Evaporate/Reconstitute 0.2 ml 25:75 acetonitrile/buffer (25 mm ammonium formate ph 4.5) add 0.25 ml 200 mm ammonium formate in 50:50 ACN/methanol* * buffers sample to protect acid labile analytes 2011 Waters Corporation 18
19 Effect of Buffering Prior to Evaporation Analyte Recovery Without Buffer Recovery With Buffer Sulfamerizine Lincomycin < Erythromycin < Penicillin < Waters Corporation 19
20 Results: Milk 0.67 x MRL Level Compound MRL Spiked %REC (%RSD) %Suppression Level (ppb) n=3 Carbadox (27)* 43 (enhance) Chloramphenicol(P) (16) 10.0 Chlorotetracyline (T) (20) 7.0 Ciprofloxacin (F) (20) 32.0 Dexamethasone (St) (6) 8 (enhance) Enrofloxacin (F) (11) 26.0 Erythromycin (M) (10) 5.0 Lincomycin(M) (9) 25.0 Oxacillin (B-L) (12) 9 (enhance) Oxytetracycline (T) (16) 9 (enhance) Penicillin (B-L) (8) 8(enhance) Phenylbutazone (NSAID) (18) 20.0 Ractopamine (14) 0.0 Salbutamol (3) 96.0 Sulfamerazine (S) (4) 16 (enhance) Sulfamethazine (S) (6) 74 (enhance) Sulfanilamide (S) (30)* 60.0 Tetracycline (T) (18) 21 (enhance) * Response Near Detection Limit 2011 Waters Corporation 20
21 Part 2 Pork Muscle Analysis 2011 Waters Corporation 21
22 Pork Muscle Composition Typical Pork Muscle Approximately 30 % solids o 5-20 % fat o % protein o ~70% water 2011 Waters Corporation 22
23 Analytical Method For This Study Pork Muscle 5 g Sample Extraction/Precipitation Weigh homogenized sample into 50 ml centrifuge tube Add 10 ml of 0.2 % formic acid in 80:20 ACN/water Vortex, shake 30 min x g Take 0.60 ml supernatant provides good recovery of most compounds much fat in extract SPE Cleanup Sep-Pak tc18 (40 mg 96 well plate) Evaporate and reconstitute 2011 Waters Corporation 23
24 SPE Cleanup Sep-Pak tc18 Plate (pass-thru mode) Condition 500 µl 80:20 acetonitrile/water Pass-Thru/Collect 600 µl sample extract install collection plate 40 mg/well Rinse/Collect 600 µl 80:20 acetonitrile/water Evaporate/Reconstitute 250 µl 20:80 acetonitrile/water add 200 μl 200 mm ammonium formate in 50:50 ACN/methanol* * buffers sample to protect acid labile analytes 2011 Waters Corporation 24
25 Results: Pork Muscle 1 x MRL Level Compound MRL Spiked %REC (%RSD) %Suppression Level (ppb) n=5 Carbadox (36)* 62.7 Chloramphenicol(P) (20) 7.1 Chlorotetracyline (T) (11) 5.7 Ciprofloxacin (F) (21) 85.6 Dexamethasone (St) (7) 36.9 Enrofloxacin (F) (4) 70.3 Erythromycin (M) (9) 4.2 Lincomycin(M) (17) 93.4 Oxacillin (B-L) (4) 25.2 Oxytetracycline (T) (8) 9.4 Penicillin (B-L) (7) 11.3 Phenylbutazone (NSAID) (16) 53.3 Ractopamine (7) 81.1 Salbutamol (14) 97.4 Sulfamerazine (S) (5) 56.7 Sulfamethazine (S) (5) 53.6 Sulfanilamide (S) (21)* 71.8 Tetracycline (T) (10) 0.4 Tylosin (11) 8.4 * Response Near Detection Limit 2011 Waters Corporation 25
26 Conclusions Sample Preparation Methods were demonstrated for determination of multiclass/multiresidue veterinary drugs in milk and meat A two step extraction/protein precipitation procedure was demonstrated for milk analysis Recoveries averaged 67% (22-110) with the lowest values for tetracyclines Matrix effects, though significant, were less than for meat samples A single step meat extraction/protein precipitation procedure was evaluated Recoveries averaged 60% (9-106) with the lowest values for carbadox and phenyl butazone Matrix effects were significant 2011 Waters Corporation 26
27 Conclusions Sample Cleanup Pass-thru cleanup using C18-silica was used in this study Effective for removal of residual fats from both types of extracts Not effective for reduction of matrix effects There is much opportunity for development of improved cleanup procedures for these types of analysis 2011 Waters Corporation 27
28 Thank s for your attention! 2011 Waters Corporation 28
Determination, Confirmation and Quantitation of Multi-Class Antibiotic Residues in Milk by UHPLC MS/MS
APPLICATION NOTE Liquid Chromatography/ Mass Spectrometry Authors: Avinash Dalmia PerkinElmer, Inc. Shelton, CT Determination, Confirmation and Quantitation of Multi-Class Antibiotic Residues in Milk by
More informationQuantification of Chloramphenicol in Chicken Using Xevo TQD with RADAR Technology
Quantification of Chloramphenicol in Chicken Using Xevo TQD with RADAR Technology Dimple Shah, Marian Twohig, and Jennifer A. Burgess Waters Corporation, Milford, MA, U.S.A. A P P L I C AT ION B E N E
More information[ APPLICATION NOTE ] Analysis of Ketamine and Xylazine in Rat Tissues Using the ACQUITY UPLC with 2D Technology APPLICATION BENEFITS INTRODUCTION
Analysis of Ketamine and Xylazine in Rat Tissues Using the ACQUITY UPLC with 2D Technology Malorie Mella, 2 Brendan Schweitzer, 1 Sabra R. Botch-Jones, M.S., M.A, 1 Claude R. Mallet, Ph.D. 2 Boston University
More informationOasis PRiME HLB Food Applications Notebook
Oasis PRiME HLB Food Applications Notebook SCIENTIST BIOS Michael S. Young, Ph.D. Principal Applications Chemist Waters Corporation Dr. Young is a Principal Chemist and Applications Manager in the Scientific
More informationUltra-Fast Analysis of Contaminant Residue from Propolis by LC/MS/MS Using SPE
Ultra-Fast Analysis of Contaminant Residue from Propolis by LC/MS/MS Using SPE Matthew Trass, Philip J. Koerner and Jeff Layne Phenomenex, Inc., 411 Madrid Ave.,Torrance, CA 90501 USA PO88780811_L_2 Introduction
More informationVeterinary Drug Detection in Pork and Milk
Application Note Food Testing Veterinary Drug Detection in Pork and Milk Using an Ultivo LC/TQ with a standard ESI ion source Figure 1. Agilent Ultivo LC/TQ with ESI source. Author Theresa Sosienski Agilent
More informationOasis PRiME HLB - Introducing A New Sorbent for the Sample Cleanup of Food Matrices
Oasis PRiME HLB - Introducing A New Sorbent for the Sample Cleanup of Food Matrices Thank you for joining us! Our Webinar will begin shortly. While you are waiting, please feel free to browse our library
More informationScreening 36 Veterinary Drugs in Animal Origin Food by LC/MS/MS Combined with Modified QuEChERS Method
Screening 36 Veterinary Drugs in Animal Origin Food by LC/MS/MS Combined with Modified QuEChERS Method Application Note Food Testing and Agriculture Authors Jin-Lan Sun, Chang Liu, Yue Song Agilent Technologies
More informationRapid LC-MS/MS Method for the Analysis of Fipronil and Amitraz Insecticides and Associated Metabolites in Egg and Other Poultry Products
Rapid LC-MS/MS Method for the Analysis of Fipronil and Amitraz Insecticides and Associated Metabolites in Egg and Other Poultry Products Ashley Sage 1, Jianru Stahl-Zeng 2, Jason Causon 1, Mike Whitmore
More informationAnalysis of Multiclass Veterinary Drugs in Baby Food by Ultra Fast Chromatography with High Performance Triple Quadrupole Mass Spectrometry
Analysis of Multiclass Veterinary Drugs in Baby Food by Ultra Fast Chromatography with High Performance Triple Quadrupole Mass Spectrometry Charles Yang, 1 Dipankar Ghosh, 1 Mary Blackburn, 1 Jamie Humphries
More informationMulti-residue Screening of Veterinary Drugs (I) and (II) in Meat According to the Japan Positive List Using Cartridge-based SPE and LC-MS/MS
Multi-residue Screening of Veterinary Drugs (I) and (II) in Meat According to the Japan Positive List Using Cartridge-based SPE and LC-MS/MS Application Note Food & Agriculture Authors Eugene Chang, Kazuyuki
More informationDetermination of Benzimidazole Residues in Animal Tissue by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry
PO-CON1472E Determination of Benzimidazole Residues in Animal Tissue by Ultra High Performance Liquid Chromatography Tandem ASMS 14 TP 21 Yin Huo, Jinting Yao, Changkun Li, Taohong Huang, Shin-ichi Kawano,
More informationOne Analysis, One Column, Less than 9 Minutes for Over 60 Multiclass Antibiotics
Featured Application: Multiclass Veterinary Antibiotics on Raptor C8 by LC- One Analysis, One Column, Less than 9 Minutes for Over 0 Multiclass Antibiotics Highly efficient peak separation and fast analysis
More informationSensitive and selective analysis of fipronil residues in eggs using Thermo Scientific GC-MS/MS triple quadrupole technology
APPLICATION NOTE 10575 Sensitive and selective analysis of fipronil residues in eggs using Thermo Scientific GC-MS/MS triple quadrupole technology Authors Cristian Cojocariu, 1 Joachim Gummersbach, 2 and
More informationANTIBIOTICS RESIDUES IN HONEY: VALIDATION PROCEDURE HONEY ANALYTICAL METHODS VALIDATION
APIACTA 40 (2005) PAGE 45-49 - 45 - ANTIBIOTICS RESIDUES IN HONEY: VALIDATION PROCEDURE HONEY ANALYTICAL METHODS VALIDATION Albino Gallina, Cristiana Benetti, Giancarlo Biancotto, Alessandra Baggio, Chiara
More informationStability of Tylosin in Honey Impact on Residue Analysis Don Noot, Tom Thompson
Stability of Tylosin in Honey Impact on Residue Analysis Don Noot, Tom Thompson Background Information collaboration with Agriculture and Agri-Food Canada project leader: Dr. Steve Pernal (Beaverlodge,
More informationMulti-residue Determination of Polar Veterinary Drugs in Livestock and Fishery Products by Liquid Chromatography/ Tandem Mass Spectrometry
23 Kanda et al.: Journal of AOAC International Vol. 98, No. 1, 215 VETERINARY DRUG RESIDUES Multi-residue Determination of Polar Veterinary Drugs in Livestock and Fishery Products by Liquid Chromatography/
More informationMulti-residue Method II for Veterinary Drugs by HPLC (Animal and Fishery Products)
Multi-residue Method II for Veterinary Drugs by HPLC (Animal and Fishery Products) 1. Analytes See Table 8. 2. Instruments High performance liquid chromatograph-photodiode array detector (HPLC-DAD) High
More informationAnalysis of Hormones & Anabolics
Analysis of Hormones & Anabolics Hormones and anabolics can be used as growth promoters in livestock breeding to enhance average daily weight gain and meat/fat ratio. As a consequence, hormone and anabolic
More informationChemical Residue Testing and the Role of Proficiency Testing Material at the Centre for Veterinary Drug Residues
2014/SCSC/WKSP2/003 Session: 5.1 Chemical Residue Testing and the Role of Proficiency Testing Material at the Centre for Veterinary Drug Residues Submitted by: Canada Food Safety Cooperation Forum Partnership
More informationAccepted Manuscript. Authors: Meritxell Gros, Sara Rodríguez-Mozaz, Damià Barceló
Title: Rapid analysis of multiclass antibiotic residues and some of their metabolites in hospital, urban wastewater and river water by ultra-high-performance liquid chromatography coupled to quadrupole-linear
More informationQuantitative and confirmatory analysis of veterinary drug residues in food of animal origin by UPLC- MS/MS after QuEChERS clean-up
Quantitative and confirmatory analysis of veterinary drug residues in food of animal origin by UPLC- MS/MS after QuEChERS clean-up Michelle Whelan 1,2 Martin Danaher 1, Ambrose Furey 2. Ashtown Food Research
More informationA Unique Approach to Managing the Problem of Antibiotic Resistance
A Unique Approach to Managing the Problem of Antibiotic Resistance By: Heather Storteboom and Sung-Chul Kim Department of Civil and Environmental Engineering Colorado State University A Quick Review The
More informationAn LC-MS/MS method to determine antibiotic residues in distillers grains
An LC-MS/MS method to determine antibiotic residues in distillers grains Hemakanthi de Alwis FDA Center for Veterinary Medicine Office of Research 07-31-2018 Distillers grain (DG) q DG is a major co-product
More informationQuantification of EPA 1694 Pharmaceuticals and Personal Care Products in Water at the ng/l Level Utilizing Online Sample Preparation with LC-MS/MS
Application Note: 58 Key Words EQuan System TSQ Vantage PPCPs Water Analysis Quantification of EPA 1694 Pharmaceuticals and Personal Care Products in Water at the ng/l Level Utilizing Online Sample Preparation
More informationAutomated Online Multi-Residue LC-MS/MS Method for the Determination of Antibiotics in Chicken Meat
Automated Online Multi-Residue LC-MS/MS Method for the Determination of Antibiotics in Chicken Meat Katerina Bousova, Klaus Mittendorf, Thermo Fisher Scientific Food Safety Response Center, Dreieich, Germany
More informationDetection of residues of quinolones in milk
Food Safety and Monitoring of Safety Aspects 77 Detection of residues of quinolones in milk Gertraud Suhren and P. Hammer Federal Dairy Research Centre, Institute for Hygiene, Hermann-Weigmann-Str. 1,
More informationMulti-residue Method I for Veterinary Drugs by HPLC (Animal and Fishery Products)
Multi-residue Method I for Veterinary Drugs by HPLC (Animal and Fishery Products) 1. Analytes See Table 7. 2. Instruments High performance liquid chromatograph-photodiode array detector (HPLC-DAD) High
More informationC 22 H 28 FNa 2 O 8 Pıı516.4
SIMULTANEOUS DETERMINATION OF DEXAMETHASONE SODIUM PHOSPHATE AND CHLORAMPHENICOL IN OPHTHALMIC SOLUTIONS W.A. Shadoul, E.A. Gad Kariem, M.E. Adam, K.E.E. Ibrahim* Department of Pharmaceutical Chemistry,
More informationMulti-residue Automated Turbulent Flow Online LC-MS/MS Method for the Determination of Antibiotics in Milk
Multi-residue Automated Turbulent Flow Online LC-MS/MS Method for the Determination of Antibiotics in Milk Katerina Bousova, Klaus Mittendorf, Thermo Fisher Scientific Food Safety Response Center, Dreieich,
More informationFluoroquinolones ELISA KIT
Fluoroquinolones ELISA KIT Cat. No.:DEIA6883 Pkg.Size:96T Intended use The Fluoroquinolones ELISA KIT is an immunoassay for the detection of Fluoroquinolones in contaminated samples including water, fish
More informationInternational Journal of Pharmacy and Pharmaceutical Sciences. Research Article
Academic Sciences International Journal of Pharmacy and Pharmaceutical Sciences ISSN- 0975-1491 Vol 4, Suppl 3, 2012 Research Article A NOVEL AND HIGH-THROUGHPUT METHOD FOR THE SIMULTANEOUS DETERMINATION
More informationValidation of bee4sensor for Honey
Conffidence Workshop: Work package 2b - Antibiotics Detection, analysis and control of veterinary pharmaceuticals in food and feed Validation of bee4sensor for Honey EuroResidue VII 16 May 2012 Hotel Zuiderduin,
More informationANTIBIOTICS IN PLASMA
by LC/MS Code LC79010 (Daptomycin, Vancomycin, Streptomycin, Linezolid, Levofloxacin, Ciprofloxacin, Gentamicin, Amikacin, Teicoplanin) INTRODUCTION Technically it defines "antibiotic" a substance of natural
More informationAnalysis of Veterinary Drugs in Meat with the Agilent 6495 Triple Quadrupole LC/MS
Analysis of Veterinary Drugs in Meat with the Agilent 6495 Triple Quadrupole LC/MS Application Note Food Authors Tarun Anumol, Joan M. Stevens, and Jerry Zweigenbaum Agilent Technologies Inc. Abstract
More informationJournal of Applied Pharmaceutical Research ISSN No
SIMULTANEOUS ESTIMATION OF PYRANTEL PAMOATE, PRAZIQUANTEL & FEBANTEL BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY USING DUAL WAVELENGTH Rupali Sajjanwar (Rupali Jitendra Paranjape)*, Shyamala Bhaskaran, Kulesh
More informationCOMMITTEE FOR VETERINARY MEDICINAL PRODUCTS
The European Agency for the Evaluation of Medicinal Products Veterinary Medicines Evaluation Unit EMEA/MRL/389/98-FINAL July 1998 COMMITTEE FOR VETERINARY MEDICINAL PRODUCTS ENROFLOXACIN (extension to
More informationIntroduction PAPER IN FOREFRONT. Larissa J. M. Jansen 1 & Yvette J. C. Bolck 1 & Janneau Rademaker 1 & Tina Zuidema 1 & Bjorn J. A.
Anal Bioanal Chem (2017) 409:4927 4941 DOI 10.1007/s00216-017-0445-0 PAPER IN FOREFRONT The analysis of tetracyclines, quinolones, macrolides, lincosamides, pleuromutilins, and sulfonamides in chicken
More informationAnalysis of Contaminants in Food
Seminar on Contaminants in Food FSAI 17 th November 2009 Analysis of Contaminants in Food Michael O Keeffe Scientific Committee FSAI Analysis of Contaminants in Food Residue analysis what is involved?
More informationJournal of Integrative Agriculture 2018, 17(6): Available online at ScienceDirect
Journal of Integrative Agriculture 2018, 17(6): 1234 1240 Available online at www.sciencedirect.com ScienceDirect RESEARCH ARTICLE Elimination of ceftiofur hydrochloride residue in postpartum cows milk
More informationThe development of a new multiplex dipstick for the simultaneous detection of sulfonamides, (fluoro)quinolones, tylosin and chloramphenicol in honey
The development of a new multiplex dipstick for the simultaneous detection of sulfonamides, (fluoro)quinolones, tylosin and chloramphenicol in honey Stefan Weigel (RIKILT), Vincent Chabottaux (Unisensor)
More informationA validated UPLC/ESI-MS/MS bioanalytical method for the quantification of Perindopril and Amlodipine in human plasma. Kalaiyarasi.
A validated UPLC/ESI-MS/MS bioanalytical method for the quantification of Perindopril and Amlodipine in human plasma Kalaiyarasi. D JNTU, Hyderabad Scope of the Method Validation Encompasses all possible
More informationOccurrence of Antibiotics in Drinking Water
Occurrence of Antibiotics in Drinking Water Zhengqi Ye, Howard S. Weinberg Michael T. Meyer U. S. Geological Survey, Kansas Abstract The occurrence of antibiotics in the aquatic environment has raised
More informationIJCBS, 10(2016): International Journal of Chemical and Biochemical Sciences (ISSN )
IJCBS, 10(2016):10-15 International Journal of Chemical and Biochemical Sciences (ISSN 2226-9614) Journal Home page: www.iscientific.org/journal.html International Scientific Organization Quantification
More informationMultilaboratory Trial for Determination of Ceftiofur Residues in Bovine and Swine Kidney and Muscle, and Bovine Milk
30 HORNISH ET AL.: JOURNAL OF AOAC INTERNATIONAL VOL. 86, NO. 1, 2003 DRUGS, COSMETICS, FORENSIC SCIENCES Multilaboratory Trial for Determination of Ceftiofur Residues in Bovine and Swine Kidney and Muscle,
More informationAntibiotics Removal in Biological Sewage Treatment Plants
DOI: 10.7508/pj.2016.02.003 Print ISSN 2383-451X Online ISSN: 2383-4501 Web Page: https://jpoll.ut.ac.ir Email: jpoll@ut.ac.ir Antibiotics Removal in Biological Sewage Treatment Plants Ghosh, G.C. 1,2*,
More informationDEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF ALISKIREN AND AMLODIPINE IN TABLET DOSAGE FORM
Page288 Research Article Pharmaceutical Sciences DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF ALISKIREN AND AMLODIPINE IN TABLET DOSAGE FORM Divya P, Aleti P, Venisetty
More informationVALIDATED RP-HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF AMLODIPINE BESYLATE AND ATORVASTATIN CALCIUM IN BULK AND PHARMACEUTICAL FORMULATION
INTERNATIONAL JOURNAL OF RESEARCH IN PHARMACY AND CHEMISTRY Available online at www.ijrpc.com Research Article VALIDATED RP-HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF AMLODIPINE BESYLATE AND ATORVASTATIN
More informationDeborah A. Cera - Division of Compliance Center for Veterinary Medicine, FDA
Deborah A. Cera - Division of Compliance Center for Veterinary Medicine, FDA 1 1 Databases RVIS Interagency Database TRIMS An Interactive Database Containing Information Obtained During FDA/State Inspections
More informationSchedule of Accreditation issued by United Kingdom Accreditation Service 2 Pine Trees, Chertsey Lane, Staines-upon-Thames, TW18 3HR, UK
2 Pine Trees, Chertsey Lane, Staines-upon-Thames, TW18 3HR, UK Minerva House Unit 2 Stoney Gate Road Spondon Derbyshire DE21 7RY Contact: Mr Ian Brown Tel: +44 (0)1332 890384 Fax: +44 (0)1332 666040 E-Mail:
More informationAMOXICILLIN AND CLAVULANIC ACID TABLETS Draft proposal for The International Pharmacopoeia (February 2018)
February 2018 Draft for comment 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 AMOXICILLIN AND CLAVULANIC ACID TABLETS Draft
More informationQuantification of Several Acidic Drugs in Equine Serum Using LC MS-MS
Journal of Analytical Toxicology Advance Access published August 27, 2013 Journal of Analytical Toxicology 2013;1 5 doi:10.1093/jat/bkt069 Special Issue Quantification of Several Acidic Drugs in Equine
More informationPHARMA SCIENCE MONITOR AN INTERNATIONAL JOURNAL OF PHARMACEUTICAL SCIENCES PHARMACOKINETIC INTERACTION OF MOXIFLOXACIN AND
PHARMA SCIENCE MONITOR AN INTERNATIONAL JOURNAL OF PHARMACEUTICAL SCIENCES PHARMACOKINETIC INTERACTION OF MOXIFLOXACIN AND MELOXICAM FOLLOWING INTRAMUSCULAR ADMINISTRATION IN RATS KA Sadariya, AK Gothi,
More informationDevelopment of Analytical Methods for the Determination of Flunixin and Phenylbutazone Drug Residues in Edible Bovine Tissues
Development of Analytical Methods for the Determination of Flunixin and Phenylbutazone Drug Residues in Edible Bovine Tissues Philip Asea, John Patterson, & Joe Boison CVDR, Health of Animals Laboratory,
More informationRevolutionary Milk Analysis
Revolutionary Milk Analysis 2 Milk quality is a major concern Farmers, producers and laboratories have to meet European and international rules. They must perform even more stricter controls to ensure
More informationAvoiding residues and an FDA Inspection
Avoiding residues and an FDA Inspection James D. McKean, DVM, JD Extension Veterinarian Associate Director, Iowa Pork Industry Center Iowa State University x2mckean@iastate.edu USDA FSIS Residue Testing
More informationDetermination of Acaricides in Korean Honey Bull. Korean Chem. Soc. 2008, Vol. 29, No
Determination of Acaricides in Korean Honey Bull. Korean Chem. Soc. 2008, Vol. 29, No. 5 1043 Simultaneous Determination of Amitraz, Bromopropylate, Coumaphos, Cymiazole and 2,4-Dimethylaniline in Korean
More informationShould you have any questions, please contact Edith Chang, Ph.D., Senior Scientific Liaison ( or
Amlodipine and Tablets Type of Posting Posting Date Targeted Official Date Notice of Intent to Revise 26 Oct 2018 To Be Determined, Revision Bulletin Expert Committee Chemical Medicines Monographs 2 In
More informationMulti-residue Determination of Polar Veterinary Drugs in Livestock and Fishery Products by
Multi-residue Determination of Polar Veterinary Drugs in Livestock and Fishery Products by Liquid Chromatography/Tandem Mass Spectrometry Maki Kanda, Takayuki Nakajima, Hiroshi Hayashi, Tsuneo Hashimoto,
More informationCurrent EU Antibiotic Maximum Residue Limits
R-Biopharm Rhône Current EU Antibiotic Maximum Residue Limits March 2011 R-Biopharm Rhône Current EU Antibiotic Limits 2 Contents Antibiotics in Food Aminoglycosides...4 Ansamycins...4 Beta-lactams...5
More informationCompliance. Should you have any questions, please contact Praveen Pabba, Ph.D., ( or
Doxycycline Hyclate Delayed-Release Tablets Type of Posting Revision Bulletin Posting Date 28 Jul 2017 Official Date 01 Aug 2017 Expert Committee Chemical Medicines Monographs 1 Reason for Revision Compliance
More informationStreptomycin Sulfate According to USP
Application Note Antibiotics The most reliable LC-EC applications for Antibiotics analysis Aminoglycosides Amikacin Framycetin Sulphate Gentamicin Sulphate Kanamycin Sulphate Lincomycin Neomycin Spectinomycin
More informationJournal of Global Trends in Pharmaceutical Sciences
An Elsevier Indexed Journal ISSN-2230-7346 Journal of Global Trends in Pharmaceutical Sciences A NEW IMPROVED RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF HYDROCHLOROTHIAZIDE, AMLODIPINE BESYLATE AND
More informationLC-MS/MS Methods for the Effective Control of Veterinary Drugs in Raw Materials and Manufactured Products. A Food Industry Perspective
LC-MS/MS Methods for the Effective Control of Veterinary Drugs in Raw Materials and Manufactured Products. A Food Industry Perspective Thomas Bessaire, Adrienne Tarres, Andrea Beck, Claudia Mujahid, Marie-Claude
More informationMethods development to detect antibiotic activity in water samples
Methods development to detect antibiotic activity in water samples Stefan Kools (Grontmij AquaSense) Marta Wilgosz (Grontmij AquaSense, WUR) Evertjan van de Brandhof (RIVM) Gerard Stroomberg (Waterdienst)
More informationMedically Important Antibiotics in Animal Agriculture
Medically Important Antibiotics in Animal Agriculture Craig Lewis, DVM MPH Office of the Director Center for Veterinary Medicine Farm Foundation Antimicrobial Stewardship Workshop Davis, California October,
More informationProficiency study for macrolides in porcine tissue
Project number: 87.036.01 Project title: NRL tasks, residues in animal products BAS-number: WOT-0-438-III-05 Project leader: mrs A.A.M. Stolker Report 009.003 May 009 Proficiency study for macrolides in
More informationDevelopment and Validation of Amlodipine Impurities in Amlodipine Tablets Using Design Space Computer Modeling
American Journal of Analytical Chemistry, 2016, 7, 918-926 http://www.scirp.org/journal/ajac ISSN Online: 2156-8278 ISSN Print: 2156-8251 Development and Validation of Amlodipine Impurities in Amlodipine
More informationDevelopment and Validation of RP-HPLC Method for Determination of Related Substances of Medetomidine in Bulk Drug
Human Journals Research Article July 2016 Vol.:6, Issue:4 All rights are reserved by Nuzhath Fathima et al. Development and Validation of RP-HPLC Method for Determination of Related Substances of Medetomidine
More informationMULTI-CLASS PROCEDURE FOR ANALYSIS OF ANTIBACTERIAL COMPOUNDS IN EGGS BY LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY
Bull Vet Inst Pulawy 56, 321-327, 2012 DOI: 10.2478/v10213-012-0057-6 MULTI-CLASS PROCEDURE FOR ANALYSIS OF ANTIBACTERIAL COMPOUNDS IN EGGS BY LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY TOMASZ BŁĄDEK,
More informationDEVELOPMENT AND VALIDATION OF AMOXICILLIN AND CLAVULANATE BY USING LC-MS METHOD
WORLD JOURNAL OF PHARMACY AND PHARMACEUTICAL SCIENCES Parijatha et al. SJIF Impact Factor 6.041 Volume 6, Issue 1, 1540-1554 Research Article ISSN 2278 4357 DEVELOPMENT AND VALIDATION OF AMOXICILLIN AND
More informationSurvey Results for Method Needs
Survey Results for Method Needs Kristi McCallum, CO Louise Ogden, MN {LM} Sharon Webb, UK-DRS 2017 Annual Summer AAFCO Laboratory Methods and Services Committee Why and When? Backlog of methods needs when
More informationDetermination of ofloxacin in bulk drug and pharmaceutical dosage form by high performance liquid chromatography method
Available online at www.scholarsresearchlibrary.com Scholars Research Library Der Pharmacia Lettre, 2015, 7 (10):188-192 (http://scholarsresearchlibrary.com/archive.html) ISSN 0975-5071 USA CODEN: DPLEB4
More informationAvailable online at
Downloaded from pbr.mazums.ac.ir at 4:8 +040 on Thursday July 6th 08 [ DOI: 0.8869/acadpub.pbr...47 ] Original Article Pharmaceutical and Biomedical Research Liquid chromatography tandem mass spectrometry
More informationUnder the supervision of Dr. José Barbosa Torralbo and Dra. Dolores Barrón Bueno in Department of Analytical Chemistry at University of Barcelona
M ulti Class, M ulti Residue Method for Determination of Penicillins, Cephalosporins and Q uinolones in Cow M ilk and Validation in Accordance with Commission Decision 2002/657/E C European M asters in
More informationCountry Report: Malaysia
Country Report: Malaysia Akma Ngah Hamid Director Central Region Veterinary Laboratory (CRVL) Dpt. of Veterinary Service Introduction Antimicrobials are essential drugs and used in human and veterinary
More informationAccepted Manuscript. Andreia Freitas, Jorge Barbosa, Fernando Ramos. S (13) DOI: /j.idairyj Reference: INDA 3531
Accepted Manuscript Development and validation of a multi-residue and multiclass ultra-high-pressure liquid chromatography-tandem mass spectrometry screening of antibiotics in milk Andreia Freitas, Jorge
More informationResidues. Mike Apley, DVM, PhD
Residues Mike Apley, DVM, PhD Residues: It s Black and White Residues occur when detected concentrations of the marker residue are above the approved tolerance for that drug in that tissue. Residues are
More informationDevelopment and validation of a HPLC analytical assay method for amlodipine besylate tablets: A Potent Ca +2 channel blocker
Development and validation of a HPLC analytical assay method for amlodipine besylate tablets: A Potent Ca +2 channel blocker Richa Sah* and Saahil Arora 1. ISF College of Pharmacy, Moga, Punjab, India
More informationThe mission of the U.S. Department of Agriculture
ALI ET AL.: JOURNAL OF AOAC INTERNATIONAL VOL. 83, NO. 1, 2000 31 DRUGS, COSMETICS, FORENSIC SCIENCES Simultaneous Determination of Eprinomectin, Moxidectin, Abamectin, Doramectin, and Ivermectin in Beef
More informationTreball Final de Grau
Tutors Antoni Rúbies Prat Laboratori de l Agència de Salut Pública de Barcelona Mercè Granados Juan Departament de Química Analítica Treball Final de Grau Determination of non-steroidal anti-inflammatory
More informationDETERMINATION OF ACTIVE SUBSTANCES IN MULTICOMPONENT VETERINARY PREPARATIONS OF ANTIPARASITIC ACTION BY HPLC METHOD
Acta Poloniae Pharmaceutica ñ Drug Research, Vol. 67 No. 5 pp. 463ñ468, 2010 ISSN 0001-6837 Polish Pharmaceutical Society DETERMINATION OF ACTIVE SUBSTANCES IN MULTICOMPONENT VETERINARY PREPARATIONS OF
More informationUsing Charm II 7600 For Residue Testing in Meats in Barbados
Using Charm II 7600 For Residue Testing in Meats in Barbados Dr Trevor King/ June Roach, Vet Services Lab (VSL) Ministry of Agriculture & Rural Development, Barbados VSL s Client Base Poultry In dustry
More informationHPLC method for simultaneous determination of Albendazole metabolites in plasma
Available online www.jocpr.com Journal of Chemical and Pharmaceutical Research, 2014, 6(11): 860-865 Research Article ISSN : 0975-7384 CODEN(USA) : JCPRC5 HPLC method for simultaneous determination of
More informationPOST SCREENING METHODS FOR THE DETECTION OF BETA-LACTAM RESIDUES IN PIGS.
POST SCREENING METHODS FOR THE DETECTION OF BETA-LACTAM RESIDUES IN PIGS. Lorraine Lynas, Deborah Currie and John D.G. McEvoy. Department of Agriculture and Rural Development for Northern Ireland, Veterinary
More informationMOXIFLOXACIN HYDROCHLORIDE (MOXIFLOXACINI HYDROCHLORIDUM) Draft proposal for The International Pharmacopoeia. (January 2018)
January 2018 DRAFT FOR COMMENT 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 MOXIFLOXACIN HYDROCHLORIDE (MOXIFLOXACINI HYDROCHLORIDUM) Draft proposal
More informationECLIPSE 50. Test for the detection of inhibitory substances in milk
ECLIPSE 50 Test para la detección de substancias antibacterianas en leche Test for the detection of inhibitory substances in milk S.L. María de Luna 11, Nave 19 50018 Zaragoza (SPAIN) Telephone/Fax: 34
More informationDrug Use on the Farm & Antibiotic Resistance in Raw, Stored, & Treated Manures
Drug Use on the Farm & Antibiotic Resistance in Raw, Stored, & Treated Manures Jason Oliver, PhD Cornell PRO-DAIRY Dairy Environmental Systems Dairy Practices Council Annual Conference Buffalo, NY Nov.
More informationVeterinary Feed Directive
Veterinary Feed Directive Medically Important Antibiotics in Animal Agriculture Outline Questions to Be Addressed What changes are being made and why? What drugs are affected, which ones are not? What
More informationAnalytical Chemistry Insights 2014:9
pen Access: Full open access to this and thousands of other papers at http://www.la-press.com. Analytical Chemistry Insights A UPLC MS Method for the Determination of floxacin Concentrations in Aqueous
More informationOccurrence of Pharmaceuticals, Hormones, and Organic Wastewater Compounds in Pennsylvania Waters
Occurrence of Pharmaceuticals, Hormones, and Organic Wastewater Compounds in Pennsylvania Waters U.S. Geological Survey Scientific Investigations Report 2012-5106 Background Pharmaceuticals, Hormones,
More informationScreening and Identification Methods for official control of Banned Antibiotics and Growth promoters in Feedingstuffs
Screening and Identification Methods for official control of Banned Antibiotics and Growth promoters in Feedingstuffs SIMBAG FEED Competitive and sustainable growth programme (GROWTH) project G6RD-CT-2000-00413
More informationAmlodipine, Valsartan, and Hydrochlorothiazide Tablets
. Table Interim Revision Announcement Official November 1, 2017 Amlodipine 1 Amlodipine, Valsartan, and Hydrochlorothiazide Tablets 2 (Continued) Tablet Strength Nominal Amlodipine/ Nominal Concentra-
More informationDAIRY VETERINARY NEWSLETTER
DAIRY VETERINARY NEWSLETTER Drought Year Issues Include Aflatoxin Testing and Nitrate Testing of Feed Aflatoxins in corn and other feed crops during drought conditions September 2012 2012 is shaping up
More informationInternational Journal of Pharmaceutical Research & Analysis
13 International Journal of Pharmaceutical Research & Analysis e-issn: 2249 7781 Print ISSN: 2249 779X www.ijpra.com RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF AMLODIPINE
More informationAnalytica Chimica Acta 529 (2005)
Analytica Chimica Acta 529 (2005) 265 272 Validation of a liquid chromatography tandem mass spectrometric method for the quantification of eight quinolones in bovine muscle, milk and aquacultured products
More informationThe absorption, distribution, metabolism and excretion study of radiolabelled meloxicam in sheep following trans-mucosal delivery
final report Project code: P.PSH.0643 Prepared by: Fiona Cotter Troy Laboratories Pty Ltd Date published: 4 February 2016 PUBLISHED BY Meat & Livestock Australia Limited Locked Bag 991 NORTH SYDNEY NSW
More informationPremi Test. Art. No. R3900. R-Biopharm AG. Fast Determination of antibiotic residues in less than 4 hours
Premi Test Art. No. R3900 Fast Determination of antibiotic residues in less than 4 hours Easy Simple handling and no extraordinary cost intensive equipment needed Sensitive Detects antibiotic residues
More informationDEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF AMLODIPINE BESYLATE AND IRBESARTAN
Indexed in Cite Factor - Directory of International Research Journals in association with leading Universities DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF AMLODIPINE BESYLATE
More informationFlunixin is the only NSAID approved for use in cattle. Pharmacokinetics and tissue elimination of flunixin. in veal calves.
Pharmacokinetics and tissue elimination of flunixin in veal calves Lindsey W. Kissell dvm, phd Patrick D. Brinson dvm Ronette Gehring bvsc, mmed vet Lisa A. Tell dvm Scott E. Wetzlich bs Ronald E. Baynes
More information