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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 a method for the determination of triazole fungicides in wine, digestion SPME was used as enrichment and purification methods to determine triazole in wine by gas chromatography-mass spectrometry (GC-MS) Residues of fungicides. The effects of extraction mode, type of extraction head, extraction temperature, extraction time, salt effect and stirring speed on the extraction efficiency were investigated. The optimal extraction conditions were as follows: the extraction head was 85μm polyacrylate (PA), the extraction mode was immersion, the extraction temperature was 50 ℃, the extraction time was 60 min, the stirring speed was 800 r / min and the mass fraction of NaCl was 10 g / L. The detection limits of penconazole, flusilazole, diniconazole and difenoconazole were 0.020, 0.021, 0.035 and 0.012 mg / L, respectively. The linear range was 0.1-15 mg / L, and the relative standard deviations (n = 5 ) Was between 4.0% and 9.2%, the recoveries of penconazole, flusilazole, diniconazole and difenoconazole were between 92.2% and 109.6% at the concentrations of 1 mg / L and 10 mg / L, %between. The establishment of the method provided a research method and scientific basis for the detection of triazole pesticide residues in wine.