K Minakata, O Suzuki, T Kumazawa, M Asano, N Harada
{"title":"Determination of diquat in biological materials by electron spin resonance spectroscopy.","authors":"K Minakata, O Suzuki, T Kumazawa, M Asano, N Harada","doi":"10.1007/BF01261425","DOIUrl":null,"url":null,"abstract":"<p><p>An electron spin resonance (ESR) method already in use for the quantitative analysis of paraquat was applied to the analysis of diquat in blood, serum, urine, tissue homogenates and several drinks without purification of the samples. The diquat radical produced with ascorbic acid at alkaline pH was much more stable than that produced with the commonly used sodium dithionite. Radical decay in solutions covered with n-hexane was less than 5% after 60 min over a wide range of ascorbic acid concentrations. In 0.2 N NaOH solution 85% of the radicals was present even after 24 h. The limit of detection was 0.3 micrograms/ml and the required amount of sample was 0.1 ml. When both diquat and paraquat were present in a sample the diquat was first extracted with 1-butanol prior to the ESR measurement, because both species were converted to the radicals.</p>","PeriodicalId":76860,"journal":{"name":"Zeitschrift fur Rechtsmedizin. Journal of legal medicine","volume":"103 8","pages":"599-607"},"PeriodicalIF":0.0000,"publicationDate":"1990-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1007/BF01261425","citationCount":"1","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Zeitschrift fur Rechtsmedizin. Journal of legal medicine","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.1007/BF01261425","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 1
Abstract
An electron spin resonance (ESR) method already in use for the quantitative analysis of paraquat was applied to the analysis of diquat in blood, serum, urine, tissue homogenates and several drinks without purification of the samples. The diquat radical produced with ascorbic acid at alkaline pH was much more stable than that produced with the commonly used sodium dithionite. Radical decay in solutions covered with n-hexane was less than 5% after 60 min over a wide range of ascorbic acid concentrations. In 0.2 N NaOH solution 85% of the radicals was present even after 24 h. The limit of detection was 0.3 micrograms/ml and the required amount of sample was 0.1 ml. When both diquat and paraquat were present in a sample the diquat was first extracted with 1-butanol prior to the ESR measurement, because both species were converted to the radicals.
已用于百草枯定量分析的电子自旋共振(ESR)方法被应用于分析血液、血清、尿液、组织匀浆和几种饮料中的百草枯,而无需对样品进行纯化。抗坏血酸在碱性条件下产生的双魁特自由基比常用的二亚硫酸钠产生的双魁特自由基稳定得多。在广泛的抗坏血酸浓度范围内,60分钟后,正己烷覆盖的溶液中的自由基衰变小于5%。在0.2 N NaOH溶液中,即使在24小时后仍有85%的自由基存在。检测限为0.3微克/毫升,所需样品量为0.1毫升。当样品中同时存在双甘菊和百草枯时,在ESR测量之前,首先用1-丁醇提取双甘菊,因为这两种物质都转化为自由基。