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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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. |
doi_str_mv | 10.1016/j.jpba.2004.01.006 |
format | Article |
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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. The method described has been applied to a study of the pharmacokinetics of enrofloxacin and ciprofloxacin in lactating dairy cows and beef steers.</description><identifier>ISSN: 0731-7085</identifier><identifier>EISSN: 1873-264X</identifier><identifier>DOI: 10.1016/j.jpba.2004.01.006</identifier><identifier>PMID: 15030889</identifier><identifier>CODEN: JPBADA</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>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</subject><ispartof>Journal of pharmaceutical and biomedical analysis, 2004-04, Vol.35 (1), p.143-153</ispartof><rights>2004 Elsevier B.V.</rights><rights>2004 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c382t-5b0e01fbe996b40118b3501f1af87d3f68f96de6f7aaf55679872e90371011063</citedby><cites>FETCH-LOGICAL-c382t-5b0e01fbe996b40118b3501f1af87d3f68f96de6f7aaf55679872e90371011063</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/j.jpba.2004.01.006$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,780,784,3550,27924,27925,45995</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=15604469$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/15030889$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Idowu, Olutosin R.</creatorcontrib><creatorcontrib>Peggins, James O.</creatorcontrib><title>Simple, rapid determination of enrofloxacin and ciprofloxacin in bovine milk and plasma by high-performance liquid chromatography with fluorescence detection</title><title>Journal of pharmaceutical and biomedical analysis</title><addtitle>J Pharm Biomed Anal</addtitle><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.</description><subject>Analysis</subject><subject>Analytical, structural and metabolic biochemistry</subject><subject>Animals</subject><subject>Biological and medical sciences</subject><subject>Bovine milk</subject><subject>Bovine plasma</subject><subject>Calibration</subject><subject>Cattle</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Ciprofloxacin</subject><subject>Ciprofloxacin - analysis</subject><subject>Ciprofloxacin - blood</subject><subject>Enrofloxacin</subject><subject>Fluoroquinolones - analysis</subject><subject>Fluoroquinolones - blood</subject><subject>Fundamental and applied biological sciences. 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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