Simple, rapid determination of enrofloxacin and ciprofloxacin in bovine milk and plasma by high-performance liquid chromatography with fluorescence detection

A rapid and simple procedure for determination of enrofloxacin and ciprofloxacin in bovine milk and plasma is described. Protein precipitation from both milk and plasma samples was achieved by addition of acetonitrile and phosphoric acid. Acetonitrile was removed with methylene chloride, leaving enr...

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Veröffentlicht in:Journal of pharmaceutical and biomedical analysis 2004-04, Vol.35 (1), p.143-153
Hauptverfasser: Idowu, Olutosin R., Peggins, James O.
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description A rapid and simple procedure for determination of enrofloxacin and ciprofloxacin in bovine milk and plasma is described. Protein precipitation from both milk and plasma samples was achieved by addition of acetonitrile and phosphoric acid. Acetonitrile was removed with methylene chloride, leaving enrofloxacin and ciprofloxacin in the acidic aqueous extract. The aqueous extract was analyzed by high-performance liquid chromatography (HPLC) with fluorescence detection. The limit of quantitation (LOQ) for enrofloxacin and ciprofloxacin in milk was found to be 2 ng/ml. LOQ for enrofloxacin and ciprofloxacin in plasma was found to be 1 ng/ml. Linear calibration curves were obtained with correlation coefficient ( r 2) ≥0.99. Analysis of quality control (QC) samples gave results within ±10% of the nominal values. Inter-assay precision for the analysis of milk QC samples were in the ranges: 4.63–12.49% (for enrofloxacin) and 4.67–9.86% (for ciprofloxacin). Inter-assay precision for the analysis of plasma QC samples were in the ranges: 6.60–17.31% (for enrofloxacin) and 6.14–13.87% (for ciprofloxacin). Intra-assay precision for the analysis of milk QC samples were in the following ranges: 3.65–7.21% (for enrofloxacin) and 1.58–14.28% (for ciprofloxacin). Intra-assay precision for the analysis of plasma QC samples were in the following ranges: 2.17–16.95% (for enrofloxacin) and 3.31–16.31% (for ciprofloxacin). The effectiveness of protein precipitants other than phosphoric acid was investigated. The method described has been applied to a study of the pharmacokinetics of enrofloxacin and ciprofloxacin in lactating dairy cows and beef steers.
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Intra-assay precision for the analysis of milk QC samples were in the following ranges: 3.65–7.21% (for enrofloxacin) and 1.58–14.28% (for ciprofloxacin). Intra-assay precision for the analysis of plasma QC samples were in the following ranges: 2.17–16.95% (for enrofloxacin) and 3.31–16.31% (for ciprofloxacin). The effectiveness of protein precipitants other than phosphoric acid was investigated. 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Protein precipitation from both milk and plasma samples was achieved by addition of acetonitrile and phosphoric acid. Acetonitrile was removed with methylene chloride, leaving enrofloxacin and ciprofloxacin in the acidic aqueous extract. The aqueous extract was analyzed by high-performance liquid chromatography (HPLC) with fluorescence detection. The limit of quantitation (LOQ) for enrofloxacin and ciprofloxacin in milk was found to be 2 ng/ml. LOQ for enrofloxacin and ciprofloxacin in plasma was found to be 1 ng/ml. Linear calibration curves were obtained with correlation coefficient ( r 2) ≥0.99. Analysis of quality control (QC) samples gave results within ±10% of the nominal values. Inter-assay precision for the analysis of milk QC samples were in the ranges: 4.63–12.49% (for enrofloxacin) and 4.67–9.86% (for ciprofloxacin). Inter-assay precision for the analysis of plasma QC samples were in the ranges: 6.60–17.31% (for enrofloxacin) and 6.14–13.87% (for ciprofloxacin). Intra-assay precision for the analysis of milk QC samples were in the following ranges: 3.65–7.21% (for enrofloxacin) and 1.58–14.28% (for ciprofloxacin). Intra-assay precision for the analysis of plasma QC samples were in the following ranges: 2.17–16.95% (for enrofloxacin) and 3.31–16.31% (for ciprofloxacin). The effectiveness of protein precipitants other than phosphoric acid was investigated. 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Psychology</subject><subject>General pharmacology</subject><subject>HPLC</subject><subject>Medical sciences</subject><subject>Milk - chemistry</subject><subject>Molecular Structure</subject><subject>Pharmacology. Drug treatments</subject><subject>Quinolones - analysis</subject><subject>Quinolones - blood</subject><subject>Reference Standards</subject><subject>Reproducibility of Results</subject><subject>Sensitivity and Specificity</subject><subject>Spectrometry, Fluorescence - methods</subject><issn>0731-7085</issn><issn>1873-264X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2004</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNp9kUGL1TAUhYMoznP0D7iQbHQ1rTdNm7TgRgZHhQEXKrgLaXozzbNtOkk7-n6M_9V03gNnJQQCly_nnpxDyEsGOQMm3u7z_dzqvAAoc2A5gHhEdqyWPCtE-eMx2YHkLJNQV2fkWYx7AKhYUz4lZ6wCDnXd7Mifr26cB7ygQc-uox0uGEY36cX5iXpLcQreDv63Nm6ieuqocfODSTqtv3MT0tENP--BedBx1LQ90N7d9NmMwfow6skgHdztmpaYPvhRL_4m7ewP9JdbemqH1QeMBjduc2E2B8_JE6uHiC9O9zn5fvXh2-Wn7PrLx8-X768zw-tiyaoWEJhtsWlEWwJjdcurNGDa1rLjVtS2ER0KK7W2VSVkU8sCG-Ay5chA8HPy5qib_na7YlzU6JKXYdAT-jUqySTnKb0EFkfQBB9jQKvm4EYdDoqB2kpRe7WVorZSFDAF9-qvTuprO2L378mphQS8PgE6Gj3YkNJy8QEnoCzFxr07cpiyuHMYVDRuS6xzIQWmOu_-5-Mv-ZCuNQ</recordid><startdate>20040401</startdate><enddate>20040401</enddate><creator>Idowu, Olutosin R.</creator><creator>Peggins, James O.</creator><general>Elsevier B.V</general><general>Elsevier Science</general><scope>IQODW</scope><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7X8</scope></search><sort><creationdate>20040401</creationdate><title>Simple, rapid determination of enrofloxacin and ciprofloxacin in bovine milk and plasma by high-performance liquid chromatography with fluorescence detection</title><author>Idowu, Olutosin R. ; Peggins, James O.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c382t-5b0e01fbe996b40118b3501f1af87d3f68f96de6f7aaf55679872e90371011063</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2004</creationdate><topic>Analysis</topic><topic>Analytical, structural and metabolic biochemistry</topic><topic>Animals</topic><topic>Biological and medical sciences</topic><topic>Bovine milk</topic><topic>Bovine plasma</topic><topic>Calibration</topic><topic>Cattle</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Ciprofloxacin</topic><topic>Ciprofloxacin - analysis</topic><topic>Ciprofloxacin - blood</topic><topic>Enrofloxacin</topic><topic>Fluoroquinolones - analysis</topic><topic>Fluoroquinolones - blood</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>General pharmacology</topic><topic>HPLC</topic><topic>Medical sciences</topic><topic>Milk - chemistry</topic><topic>Molecular Structure</topic><topic>Pharmacology. Drug treatments</topic><topic>Quinolones - analysis</topic><topic>Quinolones - blood</topic><topic>Reference Standards</topic><topic>Reproducibility of Results</topic><topic>Sensitivity and Specificity</topic><topic>Spectrometry, Fluorescence - methods</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Idowu, Olutosin R.</creatorcontrib><creatorcontrib>Peggins, James O.</creatorcontrib><collection>Pascal-Francis</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><jtitle>Journal of pharmaceutical and biomedical analysis</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Idowu, Olutosin R.</au><au>Peggins, James O.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Simple, rapid determination of enrofloxacin and ciprofloxacin in bovine milk and plasma by high-performance liquid chromatography with fluorescence detection</atitle><jtitle>Journal of pharmaceutical and biomedical analysis</jtitle><addtitle>J Pharm Biomed Anal</addtitle><date>2004-04-01</date><risdate>2004</risdate><volume>35</volume><issue>1</issue><spage>143</spage><epage>153</epage><pages>143-153</pages><issn>0731-7085</issn><eissn>1873-264X</eissn><coden>JPBADA</coden><abstract>A rapid and simple procedure for determination of enrofloxacin and ciprofloxacin in bovine milk and plasma is described. Protein precipitation from both milk and plasma samples was achieved by addition of acetonitrile and phosphoric acid. Acetonitrile was removed with methylene chloride, leaving enrofloxacin and ciprofloxacin in the acidic aqueous extract. The aqueous extract was analyzed by high-performance liquid chromatography (HPLC) with fluorescence detection. The limit of quantitation (LOQ) for enrofloxacin and ciprofloxacin in milk was found to be 2 ng/ml. LOQ for enrofloxacin and ciprofloxacin in plasma was found to be 1 ng/ml. Linear calibration curves were obtained with correlation coefficient ( r 2) ≥0.99. Analysis of quality control (QC) samples gave results within ±10% of the nominal values. Inter-assay precision for the analysis of milk QC samples were in the ranges: 4.63–12.49% (for enrofloxacin) and 4.67–9.86% (for ciprofloxacin). Inter-assay precision for the analysis of plasma QC samples were in the ranges: 6.60–17.31% (for enrofloxacin) and 6.14–13.87% (for ciprofloxacin). Intra-assay precision for the analysis of milk QC samples were in the following ranges: 3.65–7.21% (for enrofloxacin) and 1.58–14.28% (for ciprofloxacin). Intra-assay precision for the analysis of plasma QC samples were in the following ranges: 2.17–16.95% (for enrofloxacin) and 3.31–16.31% (for ciprofloxacin). The effectiveness of protein precipitants other than phosphoric acid was investigated. The method described has been applied to a study of the pharmacokinetics of enrofloxacin and ciprofloxacin in lactating dairy cows and beef steers.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>15030889</pmid><doi>10.1016/j.jpba.2004.01.006</doi><tpages>11</tpages></addata></record>
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subjects Analysis
Analytical, structural and metabolic biochemistry
Animals
Biological and medical sciences
Bovine milk
Bovine plasma
Calibration
Cattle
Chromatography, High Pressure Liquid - methods
Ciprofloxacin
Ciprofloxacin - analysis
Ciprofloxacin - blood
Enrofloxacin
Fluoroquinolones - analysis
Fluoroquinolones - blood
Fundamental and applied biological sciences. Psychology
General pharmacology
HPLC
Medical sciences
Milk - chemistry
Molecular Structure
Pharmacology. Drug treatments
Quinolones - analysis
Quinolones - blood
Reference Standards
Reproducibility of Results
Sensitivity and Specificity
Spectrometry, Fluorescence - methods
title Simple, rapid determination of enrofloxacin and ciprofloxacin in bovine milk and plasma by high-performance liquid chromatography with fluorescence detection
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