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固相萃取净化一液相色谱串联质谱确证茶叶中的 6种乙撑双二硫代氨基甲酸盐类农药残留 | |
其他题名 | Determination of 6 Ethylenebis Dithiocarbamates Residues in Tea by Liquid Chromatography Tandem Mass Spectrometry with Solid-phase Extraction Purification |
祝伟霞; 杨冀州; 刘亚风; 魏蔚 | |
来源期刊 | 分析测试学报
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ISSN | 1004-4957 |
出版年 | 2010 |
卷号 | 29期号:11页码:1109-1113 |
中文摘要 | 建立了液相色谱串联质谱法测定茶叶中代森锌、代森锰、代森锰锌、代森钠、代森联、甲基代森锌等6种乙撑双二硫代氨基甲酸盐类农药的确证方法.方法选用碱性乙二胺四乙酸二钠作为提取液,并将难溶盐转化为水溶性钠盐,甲酯化试剂碘甲烷进行衍生化反应.采用亲水-亲脂乎衡固相萃取柱(Oasis HLB)净化甲酯化产物,甲醇洗脱,6.5 rrun内衍生物在Sunfire c_18色谱柱中完成分离,电喷雾正离子多反应监测模式下监测.茶叶中甲基代森锌的定量下限为20 mug/kg,在5~200mug/kg范围内呈良好的线性关系;其它代森盐类化合物的定量下限均为10mug/kg,在2~200mug/kg范围内呈良好的线性关系;在绿茶、红茶和乌龙茶叶中添加不同水平待测物时,平均回收率为79%~ 99%,相对标准偏差为4.7%-14.6%.经验证该方法可简单、快速、准确地检测多种茶叶中的代森与甲基代森类农药残留 |
英文摘要 | A new confirmative liquid chromatography - tandem mass spectrometric(LC - MS/MS) method was developed for the determination of six dithiocarbamate salts, including zineb, maneb, mancozeb, nabam, metiram and propineb in tea sample. The 6 analytes were extracted withan alkaline EDTA - Na_2 solution. The extracts were transformed into water-soluble sodium salt compounds and derived with organic solvent methyl iodide(CH_3I).The cleanup procedures were performed on a hydrophilic -lipophilic solid-phase extraction column(Oasis HLB SPE) and the derivative dithiocarbamates were eluted with methanol. The two derivatives were separated on a Sunfire C_18 column for 6.5 min, and analyzed quantitatively by mass spectrometry under multiple reaction monitoring (MRM) mode with positive electrospray ionization. The calibration curve for propineb had a good linearity in the range of 5 - 200 mug/kg with limit of quantitation(LOQ) of 20 mug/kg, and those for other dithiocarbamate salts were in good linearities in the range of 2- 200 mug/kg with LOQs of 10mug/kg. The recoveries for green tea, black tea and oolong tea samples at different fortified levels ranged from 79% to 99% with relative standard deviations(RSDs) of 4.7% -14.6%.The validated method was simple, fast and accurate for the quantitatively and qulitatively determination of ethylenebis and propylenebis dithiocarbarmate salts residues in different tea samples |
中文关键词 | 茶叶 ; 代森类农药 ; 二硫代氨基甲酸盐 ; 残留 ; 液相色谱串联质谱 |
英文关键词 | tea ethylenebis dithiocarbamates residues LC - MS/MS |
语种 | 中文 |
国家 | 中国 |
收录类别 | CSCD |
WOS类目 | CHEMISTRY ANALYTICAL |
WOS研究方向 | Chemistry |
CSCD记录号 | CSCD:4050275 |
资源类型 | 期刊论文 |
条目标识符 | http://119.78.100.177/qdio/handle/2XILL650/224915 |
作者单位 | 河南出入境检验检疫局, 郑州, 河南 450003, 中国 |
推荐引用方式 GB/T 7714 | 祝伟霞,杨冀州,刘亚风,等. 固相萃取净化一液相色谱串联质谱确证茶叶中的 6种乙撑双二硫代氨基甲酸盐类农药残留[J],2010,29(11):1109-1113. |
APA | 祝伟霞,杨冀州,刘亚风,&魏蔚.(2010).固相萃取净化一液相色谱串联质谱确证茶叶中的 6种乙撑双二硫代氨基甲酸盐类农药残留.分析测试学报,29(11),1109-1113. |
MLA | 祝伟霞,et al."固相萃取净化一液相色谱串联质谱确证茶叶中的 6种乙撑双二硫代氨基甲酸盐类农药残留".分析测试学报 29.11(2010):1109-1113. |
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