摘要
为建立葡萄酒中三唑类杀菌剂的测定方法,以浸入式固相微萃取技术(DI-SPME)为富集、净化手段,采用气相色谱-质谱(GC-MS)联用法检测葡萄酒中三唑类杀菌剂的残留量。考察了萃取模式、萃取头类型、萃取温度、萃取时间、盐效应和搅拌速度等因素对萃取效率的影响。最适宜的萃取条件:萃取头为85μm聚丙烯酸酯(PA)、萃取模式为浸入式、萃取温度为50℃、萃取时间为60 min、搅拌速度为800 r/min和NaCl质量分数为10 g/L。戊菌唑、氟硅唑、烯唑醇和苯醚甲环唑的检出限分别为0.020,0.021,0.035和0.012 mg/L,线性范围为0.1~15 mg/L,相对标准偏差(n=5)在4.0%~9.2%之间,添加质量浓度为1 mg/L与10 mg/L时,戊菌唑、氟硅唑、烯唑醇和苯醚甲环唑的添加回收率在92.2%~109.6%之间。方法的建立为葡萄酒中三唑类农药残留的检测提供了研究方法和科学依据。
In order to establish the determination of triazole fungicides in wine, a method of direct immersion solid-phase microextraction （DI-SPME） coupled with gas chromatography mass spectrometry （GC-MS） was developed . Various experimental parameters that affect the extraction efficiencies, such as extraction mode, fiber-coating type, extraction time, extraction temperature, salt concentration and stirring rate of the sample solution were investigated and optimized. The results showed that the optimized conditions were as follows： 85 μm PA was used, extraction mode was direct immersion, extraction temperature was 50℃, extraction time was 60 min, stirring rate was 800 r/min and concentration of NaC1 was 10 g/L. Under the optimized conditions, the detection limits obtained for ~Denconazole, flusilazole, diniconazole and difenoconazole were 0. 020, 0. 021,0. 035 and 0. 012 mg/L, respectively. The linear ranges were from 0. 1 to 15 mg/L. The relative standard deviations were between 4. 0% and 9.2% （n = 5 ） . The recoveries of the different compounds were in the range of 92. 2% - 109.6% at spiked levels of 1 mg/L and 10 mg/L. This study provides a method and theoretical foundation for analysis and evaluation triazole residues in wine.
作者
郭亚芸
史红梅
韩晓梅
张晶莹
王哲
丁燕
任凤山
GUO Ya-yun SHI Hong-mei HAN Xiao-mei ZHANG Jing-ying WANG Zhe DING Yan REN Feng-shan(Shandong Academy of Grape, Jinan 250100)
出处
《分析试验室》
CAS
CSCD
北大核心
2017年第7期811-814,共4页
Chinese Journal of Analysis Laboratory
基金
山东省自然科学基金(ZR2015YL060)资助
关键词
固相微萃取
气相色谱-质谱
三唑类杀菌剂
葡萄酒
Solid-phase microextraction
Gas chromatography mass spectrometry
Triazole fungicide
Wine
