Determination of Spectinomycin Residues in Bovine Milk Using Liquid Chromatography with Electrochemical Detection
A method capable of quantifying spectinomycin in raw bovine milk was developed and validated for 100-400 ng/mL. In this procedure the milk is centrifuged at -4 degrees C and the top fat layer removed. The defatted milk is deproteinated by precipitation with 30% trichloroacetic acid and centrifugatio...
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| Veröffentlicht in: | Journal of agricultural and food chemistry 1995-08, Vol.43 (8), p.2122-2125 |
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| container_title | Journal of agricultural and food chemistry |
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| creator | Schermerhorn, Patricia G Chu, Pak-Sin Kijak, Philip James |
| description | A method capable of quantifying spectinomycin in raw bovine milk was developed and validated for 100-400 ng/mL. In this procedure the milk is centrifuged at -4 degrees C and the top fat layer removed. The defatted milk is deproteinated by precipitation with 30% trichloroacetic acid and centrifugation. The supernatant is washed sequentially with dichloromethane, hexane, and ethyl acetate. An aliquot of the separated aqueous layer is prepared for HPLC analysis by mixing with 1-decanesulfonic acid and filtering. The analyte is separated from the matrix components using an ion-pair mobile phase and a reversed-phase column; the analyte is quantified with an electrochemical detector. Mean recoveries are 80% for milk fortified at 100 ng/mL, 76% for milk fortified at 200 ng/mL, and 77% for milk fortified at 400 ng/mL. The intralaboratory coefficients of variations are 18%, 6%, and 9%, respectively |
| doi_str_mv | 10.1021/jf00056a030 |
| format | Article |
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In this procedure the milk is centrifuged at -4 degrees C and the top fat layer removed. The defatted milk is deproteinated by precipitation with 30% trichloroacetic acid and centrifugation. The supernatant is washed sequentially with dichloromethane, hexane, and ethyl acetate. An aliquot of the separated aqueous layer is prepared for HPLC analysis by mixing with 1-decanesulfonic acid and filtering. The analyte is separated from the matrix components using an ion-pair mobile phase and a reversed-phase column; the analyte is quantified with an electrochemical detector. Mean recoveries are 80% for milk fortified at 100 ng/mL, 76% for milk fortified at 200 ng/mL, and 77% for milk fortified at 400 ng/mL. The intralaboratory coefficients of variations are 18%, 6%, and 9%, respectively</description><identifier>ISSN: 0021-8561</identifier><identifier>EISSN: 1520-5118</identifier><identifier>DOI: 10.1021/jf00056a030</identifier><identifier>CODEN: JAFCAU</identifier><language>eng</language><publisher>Washington, DC: American Chemical Society</publisher><subject>ALIMENTOS ; ANTIBIOTICOS ; ANTIBIOTIQUE ; Biological and medical sciences ; CAPTEUR ; CHROMATOGRAPHIE ; CONTAMINACION ; CONTAMINATION ; CROMATOGRAFIA ; Food industries ; Fundamental and applied biological sciences. Psychology ; LAIT ; LECHE ; Milk and cheese industries. 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Agric. Food Chem</addtitle><description>A method capable of quantifying spectinomycin in raw bovine milk was developed and validated for 100-400 ng/mL. In this procedure the milk is centrifuged at -4 degrees C and the top fat layer removed. The defatted milk is deproteinated by precipitation with 30% trichloroacetic acid and centrifugation. The supernatant is washed sequentially with dichloromethane, hexane, and ethyl acetate. An aliquot of the separated aqueous layer is prepared for HPLC analysis by mixing with 1-decanesulfonic acid and filtering. The analyte is separated from the matrix components using an ion-pair mobile phase and a reversed-phase column; the analyte is quantified with an electrochemical detector. Mean recoveries are 80% for milk fortified at 100 ng/mL, 76% for milk fortified at 200 ng/mL, and 77% for milk fortified at 400 ng/mL. The intralaboratory coefficients of variations are 18%, 6%, and 9%, respectively</description><subject>ALIMENTOS</subject><subject>ANTIBIOTICOS</subject><subject>ANTIBIOTIQUE</subject><subject>Biological and medical sciences</subject><subject>CAPTEUR</subject><subject>CHROMATOGRAPHIE</subject><subject>CONTAMINACION</subject><subject>CONTAMINATION</subject><subject>CROMATOGRAFIA</subject><subject>Food industries</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>LAIT</subject><subject>LECHE</subject><subject>Milk and cheese industries. Ice creams</subject><subject>PRODUIT ALIMENTAIRE</subject><subject>RESIDU</subject><subject>RESIDUOS</subject><subject>SENSORES</subject><issn>0021-8561</issn><issn>1520-5118</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>1995</creationdate><recordtype>article</recordtype><recordid>eNptkM1PGzEQxa2qSE2BU289-VCph2rBjtcfeyyB8qGgIpJIVS_W1GsnDtl1sDdA_nscLYo49DQjvd-8eXoIfaHkhJIhPV06QggXQBj5gAaUD0nBKVUf0YBkuVBc0E_oc0rLjCkuyQA9ntvOxsa30PnQ4uDwZG1N59vQbI1v8b1Nvt7YhPN-Fp58a_GtXz3gWfLtHI_948bXeLSIoYEuzCOsF1v87LsFvlhlmxjMwjbewArv_pjdjyN04GCV7PHbPESzXxfT0VUx_n15Pfo5LoCVVVdUhDlHFCgqacmFYFaAJEYIW9eGy3-Gl44rYFxVRNRDJZihUNUg6qqyktXsEP3ofU0MKUXr9Dr6BuJWU6J3bel3bWX6W0-vIeW4LkJrfNqfMMHZsJQZK3rMp86-7GWID1pIJrme3k30zd8_5FacXelJ5r_2vIOgYR6z5WxSyVJxVmXxey-CSXoZNrHNffw33SsODI74</recordid><startdate>19950801</startdate><enddate>19950801</enddate><creator>Schermerhorn, Patricia G</creator><creator>Chu, Pak-Sin</creator><creator>Kijak, Philip James</creator><general>American Chemical Society</general><scope>FBQ</scope><scope>BSCLL</scope><scope>IQODW</scope><scope>AAYXX</scope><scope>CITATION</scope></search><sort><creationdate>19950801</creationdate><title>Determination of Spectinomycin Residues in Bovine Milk Using Liquid Chromatography with Electrochemical Detection</title><author>Schermerhorn, Patricia G ; Chu, Pak-Sin ; Kijak, Philip James</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-a349t-903ff08a817145663e6a70c66eddc57bc54f58a358906d2863c1a9da6d99e73d3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>1995</creationdate><topic>ALIMENTOS</topic><topic>ANTIBIOTICOS</topic><topic>ANTIBIOTIQUE</topic><topic>Biological and medical sciences</topic><topic>CAPTEUR</topic><topic>CHROMATOGRAPHIE</topic><topic>CONTAMINACION</topic><topic>CONTAMINATION</topic><topic>CROMATOGRAFIA</topic><topic>Food industries</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>LAIT</topic><topic>LECHE</topic><topic>Milk and cheese industries. Ice creams</topic><topic>PRODUIT ALIMENTAIRE</topic><topic>RESIDU</topic><topic>RESIDUOS</topic><topic>SENSORES</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Schermerhorn, Patricia G</creatorcontrib><creatorcontrib>Chu, Pak-Sin</creatorcontrib><creatorcontrib>Kijak, Philip James</creatorcontrib><collection>AGRIS</collection><collection>Istex</collection><collection>Pascal-Francis</collection><collection>CrossRef</collection><jtitle>Journal of agricultural and food chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Schermerhorn, Patricia G</au><au>Chu, Pak-Sin</au><au>Kijak, Philip James</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Determination of Spectinomycin Residues in Bovine Milk Using Liquid Chromatography with Electrochemical Detection</atitle><jtitle>Journal of agricultural and food chemistry</jtitle><addtitle>J. Agric. Food Chem</addtitle><date>1995-08-01</date><risdate>1995</risdate><volume>43</volume><issue>8</issue><spage>2122</spage><epage>2125</epage><pages>2122-2125</pages><issn>0021-8561</issn><eissn>1520-5118</eissn><coden>JAFCAU</coden><abstract>A method capable of quantifying spectinomycin in raw bovine milk was developed and validated for 100-400 ng/mL. In this procedure the milk is centrifuged at -4 degrees C and the top fat layer removed. The defatted milk is deproteinated by precipitation with 30% trichloroacetic acid and centrifugation. The supernatant is washed sequentially with dichloromethane, hexane, and ethyl acetate. An aliquot of the separated aqueous layer is prepared for HPLC analysis by mixing with 1-decanesulfonic acid and filtering. The analyte is separated from the matrix components using an ion-pair mobile phase and a reversed-phase column; the analyte is quantified with an electrochemical detector. Mean recoveries are 80% for milk fortified at 100 ng/mL, 76% for milk fortified at 200 ng/mL, and 77% for milk fortified at 400 ng/mL. The intralaboratory coefficients of variations are 18%, 6%, and 9%, respectively</abstract><cop>Washington, DC</cop><pub>American Chemical Society</pub><doi>10.1021/jf00056a030</doi><tpages>4</tpages></addata></record> |
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| ispartof | Journal of agricultural and food chemistry, 1995-08, Vol.43 (8), p.2122-2125 |
| issn | 0021-8561 1520-5118 |
| language | eng |
| recordid | cdi_crossref_primary_10_1021_jf00056a030 |
| source | American Chemical Society Journals |
| subjects | ALIMENTOS ANTIBIOTICOS ANTIBIOTIQUE Biological and medical sciences CAPTEUR CHROMATOGRAPHIE CONTAMINACION CONTAMINATION CROMATOGRAFIA Food industries Fundamental and applied biological sciences. Psychology LAIT LECHE Milk and cheese industries. Ice creams PRODUIT ALIMENTAIRE RESIDU RESIDUOS SENSORES |
| title | Determination of Spectinomycin Residues in Bovine Milk Using Liquid Chromatography with Electrochemical Detection |
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