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Current Pharmaceutical Analysis

Author(s): Liya Zhou, Ping Zhang, Jiangbo Liu, Xiaobo Wu, Lei Luo, Xingran Xu* and Yonghuang Luo*

DOI: 10.2174/1573412914666181017143444

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Determination of Menbutone Residues in Edible Swine Tissues Based on Solid-Phase Extraction and RP-HPLC

Page: [159 - 167] Pages: 9

  • * (Excluding Mailing and Handling)

Abstract

Background: Menbutone is widely used as a veterinary choleretic drug in many countries. There was no publicly available analysis method for the determination of menbutone residues in swine tissues. It is necessary to establish a method to control the maximum residue limit and ensure food safety of the public.

Objective: The aim of this study is to establish an analytical method for the simultaneous determination of menbutone in muscle, fat, liver and kidney tissues from swine.

Methods: MBT residue was extracted by acetonitrile from the tissues then purified by using a C18 solid phase extraction (SPE) cartridge and an alkaline alumina (ALA) SPE cartridge. MBT was detected by RP-HPLC and separation was achieved on a Shim-pack VP-ODS C18 HPLC column using phosphoric acid solution (0.5%, v/v) and acetonitrile (45/55, v/v) at a flow rate of 1.0 mL/min. The effluent was monitored at 235 nm, and the column temperature was set to 30°C.

Results: MBT eluted at 6.3 min and no interfering peak nearby was observed. This linearity within the concentration range of 0.02 (LOQ) and 12 µg/mL (r2>0.9999, n=6). The accuracy ranged from 74.07 to 110.83% of the actual values. Intra and inter-day precision were within 15.11%. In the application study, MBT was detectable in continuously dosing MBT 10 µg/g/day to healthy swine for 7 days.

Conclusion: The proposed method has specificity, accuracy, and sensitivity, with an excellent linear relationship that successfully applied to swine tissues.

Keywords: Swine, menbutone, maximum residue limit, HPLC, method validation, solid phase extraction.

Graphical Abstract

[1]
Lund, J.; Lassen, J.B. Elimination and distribution of menbutone (Genabil®) in rats. Basic. Clin. Pharmacol., 1969, 27, 429-438.
[2]
The European Agency for the Evaluation of Medicinal Products: Committee for veterinary medicinal products menbutone summary report., ema.europa.eu/ema/(Accessed on: June 5, . 2018.
[3]
Symonds, H. The choleretic effect of menbutone and clanobutin sodium in steers. Vet. Rec., 1982, 110, 423-425.
[4]
Larska, M.; Krzysiak, M.; Smreczak, M.; Polak, M.P.; Żmudziński, J.F. First detection of Schmallenberg virus in elk (Alces alces) indicating infection of wildlife in białowieża National Park in Poland. Vet. J., 2013, 198, 279-281.
[5]
Okada, K.; Kikuchi, K.; Miura, K.; Sato, T.; Morita, Y.; Tako, M.; Ogino, T.; Kaneda, Y. Relationship between white scour of calf and alcohol stability of milk in Japanese black cattle. J. Jpn. Vet.Med. Assoc.,, 1997, 50, 74-79.
[6]
Belal, F.; El-Razeq, S.A.A.; Fouad, M.M.; Zayed, S.; Fouad, F.A. Determination of menbutone in bovine milk and meat using micellar liquid chromatography: application to injectable dosage forms. Food Anal. Methods, 2016, 9, 638-645.
[7]
Siddiqui, M.R.; Alothman, Z.A.; Rahman, N. Analytical techniques in pharmaceutical analysis: A review. Arab. J. Chem., 2017, 10, S1409-S1421.
[8]
Rahman, N.; Azmi, S.N.H.; Wu, H.F. The importance of impurity analysis in pharmaceutical products: an integrated approach. Accredit. Qual. Assur., 2006, 11, 69-74.
[9]
Alothman, Z.A.; Rahman, N.; Siddiqui, M.R. Review on pharmaceutical impurities, stability studies and degradation products: An analytical approach. Rev. Adv. Sci. Eng., 2013, 2, 155-166.
[10]
El Okle, S.O.; Tohamy, G.H.; Lebda, A.M. Evaluation of acute toxicity of genabilic acid (menbutone 10%) in rabbits. World Rabbit Sci., 2014, 22, 215-222.
[11]
Ministry of Health, Labour and Welfare: The Japanese positive list system for agricultural chemical residues in Foods. http://kensaku.mhlw.go.jp(Accessed on: June 5,. 2018.
[12]
Green, C.E.; Abraham, M.H. Investigation into the effects of temperature and stirring rate on the solid-phase extraction of diuron from water using a C18 extraction disk. J. Chromatogr. A, 2000, 885, 41-49.
[13]
Hennion, M.C. Solid-phase extraction: method development, sorbents, and coupling with liquid chromatography. J. Chromatogr. A, 1999, 856, 3-54.
[14]
Poole, C.F. New trends in solid-phase extraction. Trac-trend. Anal. Chem., 2003, 22, 362-373.
[15]
Cai, Y.; Jiang, G.; Liu, J.; Zhou, Q. Multiwalled carbon nanotubes as a solid-phase extraction adsorbent for the determination of bisphenol A, 4-n-Nonylphenol, and 4-tert-Octylphenol. Anal. Chem., 2003, 75, 2517-2521.
[16]
Xiong, J.; Li, H.; Ma, X.; You, J. Synthesis and application of a novel solid-phase extraction adsorbent for multiresidue analysis of insecticides in water. J. Sep. Sci., 2018, 41, 525-533.
[17]
Fouad, M.M.; Abdel-Razeq, S.A.; Belal, F.F.; Fouad, F.A. Spectrophotometric methods for the determination of flunixin meglumine and menbutone in bulk and dosage forms. Int. J. Phar. Anal., 2013, 4, 30-35.
[18]
Luo, Y.H.; Luo, L.; Long, F.; Wang, S.; Wang, L.Z.; Yang, Y.; Wu, M.W.; Tan, M.G. Veterinary menbutone powder and preparation method thereof. CN Patent 201,310,370,852, October 11, 2013.
[19]
Luo, Y.H.; Luo, L.; Wang, L.Z.; Yang, Y.; Long, F.; Tan, M.G.; Wang, S.; Wu, M.W. Method for determining content of veterinary menbutone injection. CN Patent 201,310,370,852 August 22, 2013.
[20]
Luo, L.; Wang, L.Z.; Luo, Y.H.; Wang, X.H.; Hu, C.H. Improved synthesis method of Menbutone. CN Patent 201,410,672,247,November 19 2014.
[21]
The People's Republic of China Announcement: Official journal:Veterinary Drug Management Regulations. http://www.gov.cn/ zwgk/2005-06/20/content_7808.htm(Accessed on: April 9,. 2004.
[22]
China Institute of Veterinary Drug Control. Veterinary drug residue testing standards operating procedures; China Agricultural Science & Technology: Beijing, 2009.
[23]
Ministry of Agriculture and Rural Affairs of the Peoples Republic of China. Announcement: Technical specification for veterinary drug residue test (trial). moa.gov.cn/govpublic/SYJ/201006/ t20100606 _1535497.html(Accessed on: January 22. 2003.
[24]
Furusawa, N. A clean and rapid liquid chromatographic technique for sulfamethazine monitoring in pork tissues without using organic solvents. J. Chromatogr. Sci., 2003, 41, 377-380.
[25]
He, L.; Wang, J.; Zhang, G.; Liu, R.; Fang, B. Simultaneous determination of tranquilizers and varazolol residues in swine tissues by liquid chromatography-tandem mass spectrometry. Anal. Lett., 2012, 45, 1377-1389.
[26]
Gumustas, M.; Sengel-Turk, C.T.; Badilli, U.; Amasya, G.; Ozkan, S.A.; Tarimci, N. Optimization of stability indicating LC method for the sensitive in vitro determination from solid lipid nanoparticles and ex vivo analysis from rat skin of etofenamate. Curr. Pharm. Anal., 2017, 13, 63-71.
[27]
Andersson, S.H.G. JanSjövall. A method combining solvent and gel extraction for isolation and preliminary purification of steroids in tissues. Anal. Biochem., 1983, 134, 309-312.
[28]
Razzaq, R.; Ranjha, N.M.; Rashid, R.; Rashid, Z.; Hanif, M. Determination of diltiazem HCL by reverse phase high performance liquid chromatography in rabbit plasma. Curr. Pharm. Anal., 2018, 14, 153-156.