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分散固相萃取超高效液相色谱法快速测定水果中的杀菌剂残留
引用本文:朱然,张倩,牛俊莉. 分散固相萃取超高效液相色谱法快速测定水果中的杀菌剂残留[J]. 广东化工, 2013, 0(23): 169-170,168
作者姓名:朱然  张倩  牛俊莉
作者单位:[1]新疆林业科学院,新疆乌鲁木齐830000 [2]新疆大学化学化工学院,新疆乌鲁木齐830046
摘    要:建立了散固相萃取超高效液相色谱法快速测定水果中的苯并咪唑类杀菌剂残留的分析方法.样品经乙腈提取后,均质离心,取上清液加入100 mg PSA及300 mg无水硫酸镁净化,离心取上清液进超高效液相色谱进行分析.对不同的色谱柱进行了选择性实验,最终采用C18柱,同时对流动相体系及净化条件进行了优化.结果:多菌灵、硫菌灵、噻菌灵、甲基硫菌灵在各自的浓度范围内呈良好的线性关系.对上述四种杀菌剂分别做3组(n=6)浓度水平的加标回收实验,平均回收率在80 %~100%之间,相对标准偏差(RSD)均小于4.41%,四种杀菌剂的检出限(LOD)分别为多菌灵、噻菌灵0.1 mg/kg,硫菌灵、甲基硫菌灵0.05 mg/kg.实验结果表明,该方法简便、快速,适合水果中残留四种杀菌剂的测定.

关 键 词:苯并咪唑  分散固相萃取  超高效液相色谱

Determination of Benzimidazole Fungicides in Fruits by PSA Dispersive Solid Phase Extraction and Ultra Performance Liquid Chromatography
Zhu Ran,Zhang Qian,Niu Junli. Determination of Benzimidazole Fungicides in Fruits by PSA Dispersive Solid Phase Extraction and Ultra Performance Liquid Chromatography[J]. Guangdong Chemical Industry, 2013, 0(23): 169-170,168
Authors:Zhu Ran  Zhang Qian  Niu Junli
Affiliation:1 (1. Xinjiang Academy of Forestry, Urumqi 830000: 2.College of Chemistry and Chemical Engineering, Xinjiang University, Urumqi 830046, China)
Abstract:A Ultra Perfom~ance Liquid Chromatography (UPLC) method had been developed for the determination of 4 benzimidazole fungicides in fruits. Alter being extracted by acetonitrile and salted-out by anhydrous magnesium sulfate, benzimidazole fungicides were partitioned into upper acetonitrile layer. 50 mg PSA and 200 mg anhydrous magnesium sulfate were added to 2 ml of the supernatant in a centrifugal tube. Fungicides were separated on a BEH-C18( 50 mmx2.1 ram, 1.7 gin), the target analyzes were separated to UPLC analysis with elution employing methanoI-H20 as mobile phase. And detection by a ultraviolet detector with the detection wavelength of 267 nm. The flow rate was 0.2 mL/min. The linear range were 0.2-10 mg/L, the coefficients of variation were not more than 4.41% and the recovery rates were 80 %-100 %. The method of Ultra Performance Liquid Chromatography introduced in this paper is simple, rapid, accurate and applicable to the analysis of fruits.
Keywords:benzimidazolefungicides  dispersive solid phase extraction: Ultra Performance Liquid Chromatography
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