摘要
建立了可用于葡萄和葡萄酒中20种唑类杀菌剂残留量的分散型固相萃取-气相色谱-正化学离子源质谱分析方法。葡萄和葡萄酒样品分别用乙腈(含1%冰醋酸)和乙酸乙酯提取,分散型固相萃取法净化,由气相色谱-正化学离子源质谱分时段选择离子监测技术进行测定与确证,外标法定量。20种农药在50～1000μg/L范围内线性均良好;所有农药的方法定量限(LOQ)均低于10μg/kg;在3个添加水平(10,20和40μg/kg)下,所有农药的回收率均处于71.2%～102.2%之间,RSD≤10.6%。
A confirmatory method was established for the determination of 20 kind of azole fungicides residues in vegetables with the technique of offline disperse solid phase extraction and gas chromatography-positive chemical ionization mass spectrometry （DSPE-GC-MS/PCI）.Pesticides interested were extracted from grape and wine with acetonitrile and ethyl acetate respectively,containing 1% acetic acid and simultaneous liquid-liquid partitioning formed by adding anhydrous magnesium sulfate plus sodium acetate following by a simple cleanup step known by dispersive solid phase extraction.The aliquot was determined and confirmed by gas chromatography-positive chemical ionization mass spectrometry （GC-MS/PCI） using external standard method.The recoveries of all pesticides were in the range from 71.2% to 102.2% at three spiked level,0.010,0.020 and 0.040 mg/kg,and the RSDs were ≤10.6%.The linearity of method was good from 50 to 1000 μg/L,and all LODs ≤10 μg/kg.The method is suitable for confirmatory of pesticides residue in grape and wine.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2010年第7期941-947,共7页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.20575027)
质检公益性行业科研专项(Nos.200810099
200810219)资助
关键词
气相色谱-正化学离子源质谱联用
选择离子监测
分散型固相萃取
唑类杀菌剂
葡萄
葡萄酒
Gas chromatography-positive chemical ionization mass spectrometry
Selected ion monitoring
Disperse solid phase extraction
Azoles fungicides
Grape
Wine
