Development and Validation of Analytical Method for Clenbuterol Chiral Determination in Animal Feed by Direct Liquid Chromatography
Tóm tắt
A direct chiral liquid chromatography with UV detection method was developed and validated for enantiomeric determination of clenbuterol β2-agonist in feed samples for poultry. To obtain optimum chromatographic conditions for chiral separation, two commercially available columns packed with vancomycin and teicoplanin chiral stationary phase (150 × 2.1 mm i.d, 5 μm) were tested. Experimental design and response surface analysis were used to model analytical responses and to get mobile phase composition for acceptable enantioresolution and performance in low analysis time. Different sample treatments based on HCX SPE and on the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method were evaluated and compared to obtain the best extraction recoveries with negligible matrix effect. Special attention was paid to compatibility between sample preparation and chiral separation to get enantioresolution and low detection limits in the high-complex sample. QuEChERS-based extraction allowed obtaining cleaner feed extracts in low sample preparation time, providing a useful and reliable method capable to control the illegal use of clenbuterol enantiomers in feed for growth promotion in food-producing animals. Reproducible recoveries, from 64 to 101 % for clenbuterol enantiomers, with relative standard deviation values within the range 1–6 %, were achieved in feed samples of poultry spiked at low concentration levels of micrograms per gram.
Tài liệu tham khảo
Abou-Basha LI, Aboul-Enein HY (1996) Biomed Chromatogr 10:69–72
Aboul-Enein HY, Serignese V (1999) Biomed Chromatogr 13:520–524
Ali I, Aboul-Enein HY (2004) Chiral pollutants: distribution, toxicity and analysis by chromatography and capillary electrophoresis. John Wiley and Sons, England
Anastassiades M, Lehotay SJ, Štajnbaher D, Schenck FJ (2003) J AOAC Int 86(2):412–431
AOAC (1998) Peer-verified methods program, manual on policies and procedures. AOAC, Arlington
AOAC (2005) 2007.01 method
Beesley TE, Lee JT (2009) J Liq Chromatogr R T 32:1733–1767
Berendsen BJA, Stolker AAM, Nielen MWF (2013) Trend Anal Chem 43:229–239
Bruzzoniti MC, Checchini L, De Carlo RM, Orlandini S, Rivoira L, Del Bubba M (2014) Anal Bioanal Chem 406:4089–4116
Cavazzini A, Pasti L, Massi A, Marchetti N, Dondi F (2011) Anal Chim Acta 706:205–222
Delgado-Zamarreño MM, Pérez-Martín L, Bustamante-Rangel M, Carabias-Martínez R (2012) Talanta 100:320–328
Du W, Lei C, Zhang S, Bai G, Zhou H, Sun M, Fu Q, Chang C (2014) J Pharm Biomed Anal 91:160–168
European Commission Decision (EC) No. 2002/657/EC of 12 (2002) Brussels, implementing council directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Off J Eur Common 1(221):8–36
Harner T, Wiberg K, Nordstrom R (2000) Environ Sci Technol 34:218–220
He L, Su Y, Zeng Z, Liu Y, Huang X (2007) Anim Feed Sci Tech 132:316–323
Hefnawy MM, Al-Shehri M, Sultan M, Mostafa GAE (2013) Dig J Nanomater Bios 8(4):1781–1790
ICH (2005) Harmonised Tripartite Guideline: validation of analytical procedures: text and methodology, Q2 (R1), Geneva
Juan C, Igualada C, Moragues F, León N, Mañes J (2010) J Chromatogr A 1217:6061–6068
Kinsella B, O’Mahony J, Malone E, Moloney M, Cantwell H, Furey A, Danaher M (2009) J Chromatogr A 1216:7977–8015
Krska R, Becalski A, Braekevelt E, Koerner T, Cao X-L, Dabeka R, Godefroy S, Lau B, Moisey J, Rawn DFK, Scott PM, Wang Z, Forsyth D (2012) Anal Bioanal Chem 402:139–162
Lammerhofer M (2010) J Chromatogr A 1217:814–856
León N, Roca M, Igualada C, Martins CPB, Pastor A, Yusá V (2012) J Chromatogr A 1258:55–65
Li J, Zhang Z, Liu X, Yan H, Han S, Zhang H, Zhang S, Cheng J (2014) Food Anal Method 7:977–985
López-Serna R, Kasprzyk-Hordern B, Petrovi M, Barceló D (2013) Anal Bioanal Chem 405:5859–5873
MacLeod SL, Sudhir P, Wong CS (2007) J Chromatogr A 1170:23–33
Martin P, Puech AJ, Brochet D, Soubrié P, Simon P (1985) Eur J Pharmacol 117:127–129
Morales-Trejo F, Vega y León S, Escobar-Medina A, Gutiérrez-Tolentino R (2013) J Food Drug Anal 21:414–420
Mostafa GAE, Hefnawy MM, El-Majed A (2009) J AOAC Inter 92(3):824–829
Park KH, Choi J, Abd El-Aty AM, Cho S, Park J, Kwon KS, Park HR, Kim HS, Shin H, Kim MR, Shim J (2012) Meat Sci 92:749–753
Pleadin J, Vuli A, Perši N, Vahi N (2010) Meat Sci 86:733–737
Prokhorova AF, Shapovalova EN, Shpigun OA (2010) J Pharm Biomed Anal 53:1170–1179
Ribeiro AR, Castro PML, Tiritan ME (2012) Environ Chem Lett 10:239–253
Song Y, Wang D, Hu Y, Chen X, Jiao Y, Hou D (2003) J Pharm Biomed Anal 31:311–319
Thevis M, Thomas A, Beuck S, Butch A, Dvorak J, Schanzer W (2013) Rapid Commun Mass SP 27(4):507–512
Van Loco J, Jànosi A, Impens S, Fraselle S, Cornet V, Degroodt JM (2007) Anal Chim Acta 586:8–12
Waldeck B, Windmark E (1985) Acta Pharmacol Toxicol 56:21–227
Wille K, De Brabander HF, De Wulf E, Van Caeter P, Janssen CR, Vanhaecke L (2012) Trend Anal Chem 35:87–108
William P, Emmanuelle V (2013) J Chromatogr A 1290:46–61
Xiu-Juan W, Feng Z, Fei D, Wei-Qing L, Qing-Yu C, Xiao-Gang C, Cheng-Bao X (2013) J Chromatogr A 1278:82–88
Zhang LY, Chang BY, Dong T, He PL, Yang WJ, Wang ZY (2009) J Chromatogr Sci 47:324–328
Zhanga M-X, Li C, Wuc Y-L (2012) J Chromatogr, B 900:94–99
Zhao L, Zhao J, Huangf W-G, Wu Y-L (2010) Chromatographia 72:365–368