M. Horie, Y. Kido, M. Murayama, M. Toyoda, H. Nakazawa
{"title":"高效液相色谱法测定肉、奶、鱼中螺旋霉素及其初级代谢物新螺旋霉素的含量","authors":"M. Horie, Y. Kido, M. Murayama, M. Toyoda, H. Nakazawa","doi":"10.3358/SHOKUEISHI.40.5_401","DOIUrl":null,"url":null,"abstract":"A simple and rapid method using HPLC for the determination of spiramycin I (major and most important component) and its metabolite, neospiramycin I, in meat, fish and milk has been developed. Neospiramycin I was obtained by acidic treatment of spiramycin I. The drugs were extracted with 1.2% metaphosphoric acid-methanol (5:5), and the extracts were cleaned up on a Bond Elut SCX (500mg) cartridge. The HPLC separation was performed on a Puresil 5C18 column (150×4.6mm i. d.) using 0.05mol/L phosphate buffer (pH 2.5) -acetonitrile (76:24) as the mobile phase at a flow rate of 0.5mL/min. The drugs were detected at 235nm. The calibration graphs were rectilinear from 2 to 50ng for both drugs. The recoveries of the drugs from meat, milk and fish at the level of 0.2μg/g were 80.3-85.3%, and detection limits were 0.05μg/g for both drugs.","PeriodicalId":17269,"journal":{"name":"Journal of The Food Hygienic Society of Japan (shokuhin Eiseigaku Zasshi)","volume":"8 1","pages":""},"PeriodicalIF":0.0000,"publicationDate":"1999-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"5","resultStr":"{\"title\":\"Determination of Spiramycin I and Its Primary Metabolite Neospiramycin I in Meat, Milk and Fish by HPLC\",\"authors\":\"M. Horie, Y. Kido, M. Murayama, M. Toyoda, H. Nakazawa\",\"doi\":\"10.3358/SHOKUEISHI.40.5_401\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"A simple and rapid method using HPLC for the determination of spiramycin I (major and most important component) and its metabolite, neospiramycin I, in meat, fish and milk has been developed. Neospiramycin I was obtained by acidic treatment of spiramycin I. The drugs were extracted with 1.2% metaphosphoric acid-methanol (5:5), and the extracts were cleaned up on a Bond Elut SCX (500mg) cartridge. The HPLC separation was performed on a Puresil 5C18 column (150×4.6mm i. d.) using 0.05mol/L phosphate buffer (pH 2.5) -acetonitrile (76:24) as the mobile phase at a flow rate of 0.5mL/min. The drugs were detected at 235nm. The calibration graphs were rectilinear from 2 to 50ng for both drugs. The recoveries of the drugs from meat, milk and fish at the level of 0.2μg/g were 80.3-85.3%, and detection limits were 0.05μg/g for both drugs.\",\"PeriodicalId\":17269,\"journal\":{\"name\":\"Journal of The Food Hygienic Society of Japan (shokuhin Eiseigaku Zasshi)\",\"volume\":\"8 1\",\"pages\":\"\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"1999-10-05\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"5\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of The Food Hygienic Society of Japan (shokuhin Eiseigaku Zasshi)\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.3358/SHOKUEISHI.40.5_401\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of The Food Hygienic Society of Japan (shokuhin Eiseigaku Zasshi)","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.3358/SHOKUEISHI.40.5_401","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
Determination of Spiramycin I and Its Primary Metabolite Neospiramycin I in Meat, Milk and Fish by HPLC
A simple and rapid method using HPLC for the determination of spiramycin I (major and most important component) and its metabolite, neospiramycin I, in meat, fish and milk has been developed. Neospiramycin I was obtained by acidic treatment of spiramycin I. The drugs were extracted with 1.2% metaphosphoric acid-methanol (5:5), and the extracts were cleaned up on a Bond Elut SCX (500mg) cartridge. The HPLC separation was performed on a Puresil 5C18 column (150×4.6mm i. d.) using 0.05mol/L phosphate buffer (pH 2.5) -acetonitrile (76:24) as the mobile phase at a flow rate of 0.5mL/min. The drugs were detected at 235nm. The calibration graphs were rectilinear from 2 to 50ng for both drugs. The recoveries of the drugs from meat, milk and fish at the level of 0.2μg/g were 80.3-85.3%, and detection limits were 0.05μg/g for both drugs.