Development of High Performance Liquid Chromatography-Tandem Mass Spectrometry Method for the Detection of Tulathromycin in Swine Plasma

doi:10.1016/S1671-2927(00)8565

Journal of Integrative Agriculture ›› 2012, Vol. 12 ›› Issue (3): 465-473.DOI: 10.1016/S1671-2927(00)8565

Development of High Performance Liquid Chromatography-Tandem Mass Spectrometry Method for the Detection of Tulathromycin in Swine Plasma

HUANG Xian-hui, LIANG Zi-sen, ZENG Zhen-ling, ZHANG Min, FANG Bing-hu

1.National Reference Laboratory of Veterinary Drug Residues, College of Veterinary Medicine, South China Agricultural University,Guangzhou 510642, P.R.China
2.Qingdao Conyinent Phaimaceutical Co. Ltd., Qingdao 266061, P.R.China

收稿日期:2011-01-10 出版日期:2012-03-01 发布日期:2012-03-11
通讯作者: Correspondence HUANG Xian-hui, Tel: +86-20-87344801, Fax: +86-20-87344801, E-mail: xhhuang@scau.edu.cn
基金资助:
This work was supported by the Guangzhou Technology Pillar Program for the Development of New Broad-Spectrum Antibiotic Tulathromycin and Industrialization during 2010, China (2010Z1-E371), and the International Communication and Cooperation for the Development of New Veterinary Medicine of Tulathromycin Raw Materials and Its Preparation, China (2010DFA32610).

Development of High Performance Liquid Chromatography-Tandem Mass Spectrometry Method for the Detection of Tulathromycin in Swine Plasma

HUANG Xian-hui, LIANG Zi-sen, ZENG Zhen-ling, ZHANG Min, FANG Bing-hu

1.National Reference Laboratory of Veterinary Drug Residues, College of Veterinary Medicine, South China Agricultural University,Guangzhou 510642, P.R.China
2.Qingdao Conyinent Phaimaceutical Co. Ltd., Qingdao 266061, P.R.China

Received:2011-01-10 Online:2012-03-01 Published:2012-03-11
Contact: Correspondence HUANG Xian-hui, Tel: +86-20-87344801, Fax: +86-20-87344801, E-mail: xhhuang@scau.edu.cn
Supported by:
This work was supported by the Guangzhou Technology Pillar Program for the Development of New Broad-Spectrum Antibiotic Tulathromycin and Industrialization during 2010, China (2010Z1-E371), and the International Communication and Cooperation for the Development of New Veterinary Medicine of Tulathromycin Raw Materials and Its Preparation, China (2010DFA32610).

摘要/Abstract

摘要： An accurate and precise method for the determination of tulathromycin in swine plasma was developed and validated. Plasma samples were analyzed by high-performance liquid chromatography with tandem mass spectrometry detection (HPLC-MS/MS) using electrospray ionization (ESI). Tulathromycin was extracted from plasma by precipitation with acetonitrile and separated using a Phenomenex Luna 5 μm C18 column (150 mm×2.0 mm) at a flow rate of 0.25 mL min-1. Solvent A consisted of 0.002 mol L-1 ammonium acetate and formic acid (999:1, v/v), and solvent B was acetonitrile. The mass spectrometer was operated in the selected-ion mode with atmospheric pressure chemical ionization to monitor the respective MH+ ions, namely, m/z 577.3 for tulathromycin and m/z 679.3 for the internal standard roxithromycin. The calibration curves were linear in a dynamic range of 2.0-500 ng mL-1 on the column. The accuracy was ranged from 95.25 to 109.75%, and the precision was ranged from 2.81 to 7.72%. The recoveries measured at 3 concentration levels (20, 250, and 500 ng mL-1) were higher than 98%. The method described above is efficient, and has the required accuracy and precision for rapid determination of tulathromycin in plasma. The method was applied to study the pharmacokinetics of tulathromycin in swine, and tulathromycin demonstrated a rapid absorption, wide distribution, and slow elimination after intramuscular administration.

关键词: tulathromycin, drug assay, pharmacokinetics, plasma, swine, HPLC-MS/MS

Abstract: An accurate and precise method for the determination of tulathromycin in swine plasma was developed and validated. Plasma samples were analyzed by high-performance liquid chromatography with tandem mass spectrometry detection (HPLC-MS/MS) using electrospray ionization (ESI). Tulathromycin was extracted from plasma by precipitation with acetonitrile and separated using a Phenomenex Luna 5 μm C18 column (150 mm×2.0 mm) at a flow rate of 0.25 mL min-1. Solvent A consisted of 0.002 mol L-1 ammonium acetate and formic acid (999:1, v/v), and solvent B was acetonitrile. The mass spectrometer was operated in the selected-ion mode with atmospheric pressure chemical ionization to monitor the respective MH+ ions, namely, m/z 577.3 for tulathromycin and m/z 679.3 for the internal standard roxithromycin. The calibration curves were linear in a dynamic range of 2.0-500 ng mL-1 on the column. The accuracy was ranged from 95.25 to 109.75%, and the precision was ranged from 2.81 to 7.72%. The recoveries measured at 3 concentration levels (20, 250, and 500 ng mL-1) were higher than 98%. The method described above is efficient, and has the required accuracy and precision for rapid determination of tulathromycin in plasma. The method was applied to study the pharmacokinetics of tulathromycin in swine, and tulathromycin demonstrated a rapid absorption, wide distribution, and slow elimination after intramuscular administration.

Key words: tulathromycin, drug assay, pharmacokinetics, plasma, swine, HPLC-MS/MS

HUANG Xian-hui, LIANG Zi-sen, ZENG Zhen-ling, ZHANG Min, FANG Bing-hu . Development of High Performance Liquid Chromatography-Tandem Mass Spectrometry Method for the Detection of Tulathromycin in Swine Plasma[J]. Journal of Integrative Agriculture, 2012, 12(3): 465-473.

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Development of High Performance Liquid Chromatography-Tandem Mass Spectrometry Method for the Detection of Tulathromycin in Swine Plasma

Development of High Performance Liquid Chromatography-Tandem Mass Spectrometry Method for the Detection of Tulathromycin in Swine Plasma

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