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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
ISSN1004-4957
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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