E. Chiavaro, A. Lepiani, F. Colla, P. Bettoni, E. Pari, E. Spotti
{"title":"免疫亲和净化和快速荧光法测定火腿中的赭曲霉毒素A","authors":"E. Chiavaro, A. Lepiani, F. Colla, P. Bettoni, E. Pari, E. Spotti","doi":"10.1080/02652030210123869","DOIUrl":null,"url":null,"abstract":"A simple and rapid method for the determination of ochratoxin A (OA) in ham was developed using a basic methanolic extraction, immunoaffinity column clean-up and a fluorometric determination of the toxin contamination levels. A mean recovery of OA from ham samples spiked at levels from 0.7 to 9.7 µg kg-1 was 83 ± 6% using the fluorometric method, with a detection limit of 0.7 µg kg-1. Recovery data were compared statistically with those obtained using reversed-phase high-performance liquid chromatography with acetonitrile-water-acetic acid (99:99:2) as mobile phase and fluorescence detection, commonly used for OA determination in food. A good correlation between the two analytical techniques was obtained. Both methods were successfully applied to 42 ham samples, 21 in the middle of the ripening period (after 6 months from the process beginning) and the other 21 at the end of the maturation, after 12 months. Twenty-seven samples (64%) showed an OA contamination level <1.0 µg kg-1, the Italian Ministry of Health guideline. The maximum contamination level found was 2.3 µg kg-1. A good agreement (R2 = 0.980) between HPLC and fluorometer analysis on naturally contaminated samples was obtained.","PeriodicalId":12310,"journal":{"name":"Food Additives & Contaminants","volume":"14 1","pages":"575 - 581"},"PeriodicalIF":0.0000,"publicationDate":"2002-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"78","resultStr":"{\"title\":\"Ochratoxin A determination in ham by immunoaffinity clean-up and a quick fluorometric method\",\"authors\":\"E. Chiavaro, A. Lepiani, F. Colla, P. Bettoni, E. Pari, E. Spotti\",\"doi\":\"10.1080/02652030210123869\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"A simple and rapid method for the determination of ochratoxin A (OA) in ham was developed using a basic methanolic extraction, immunoaffinity column clean-up and a fluorometric determination of the toxin contamination levels. A mean recovery of OA from ham samples spiked at levels from 0.7 to 9.7 µg kg-1 was 83 ± 6% using the fluorometric method, with a detection limit of 0.7 µg kg-1. Recovery data were compared statistically with those obtained using reversed-phase high-performance liquid chromatography with acetonitrile-water-acetic acid (99:99:2) as mobile phase and fluorescence detection, commonly used for OA determination in food. A good correlation between the two analytical techniques was obtained. Both methods were successfully applied to 42 ham samples, 21 in the middle of the ripening period (after 6 months from the process beginning) and the other 21 at the end of the maturation, after 12 months. Twenty-seven samples (64%) showed an OA contamination level <1.0 µg kg-1, the Italian Ministry of Health guideline. The maximum contamination level found was 2.3 µg kg-1. A good agreement (R2 = 0.980) between HPLC and fluorometer analysis on naturally contaminated samples was obtained.\",\"PeriodicalId\":12310,\"journal\":{\"name\":\"Food Additives & Contaminants\",\"volume\":\"14 1\",\"pages\":\"575 - 581\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2002-06-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"78\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Food Additives & Contaminants\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.1080/02652030210123869\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Food Additives & Contaminants","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.1080/02652030210123869","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 78
摘要
建立了一种简便、快速的测定火腿中赭曲霉毒素A (OA)的方法,采用碱甲醇提取、免疫亲和柱净化和荧光法测定毒素污染水平。采用荧光法,在0.7 ~ 9.7 μ g kg-1水平范围内,火腿样品中OA的平均回收率为83±6%,检出限为0.7 μ g kg-1。将回收率数据与常用的食品中OA测定方法——乙腈-水-乙酸(99:99:2)反相高效液相色谱法(荧光法)进行对比。两种分析方法之间具有良好的相关性。这两种方法都成功地应用于42份火腿样品,21份在成熟中期(从过程开始6个月后),另外21份在成熟末期(12个月后)。27份样品(64%)显示OA污染水平<1.0µg kg-1(意大利卫生部指南)。发现的最大污染水平为2.3µg kg-1。HPLC法与荧光法对天然污染样品的分析结果吻合良好(R2 = 0.980)。
Ochratoxin A determination in ham by immunoaffinity clean-up and a quick fluorometric method
A simple and rapid method for the determination of ochratoxin A (OA) in ham was developed using a basic methanolic extraction, immunoaffinity column clean-up and a fluorometric determination of the toxin contamination levels. A mean recovery of OA from ham samples spiked at levels from 0.7 to 9.7 µg kg-1 was 83 ± 6% using the fluorometric method, with a detection limit of 0.7 µg kg-1. Recovery data were compared statistically with those obtained using reversed-phase high-performance liquid chromatography with acetonitrile-water-acetic acid (99:99:2) as mobile phase and fluorescence detection, commonly used for OA determination in food. A good correlation between the two analytical techniques was obtained. Both methods were successfully applied to 42 ham samples, 21 in the middle of the ripening period (after 6 months from the process beginning) and the other 21 at the end of the maturation, after 12 months. Twenty-seven samples (64%) showed an OA contamination level <1.0 µg kg-1, the Italian Ministry of Health guideline. The maximum contamination level found was 2.3 µg kg-1. A good agreement (R2 = 0.980) between HPLC and fluorometer analysis on naturally contaminated samples was obtained.