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Applicability of Pressurized Liquid Extraction for Melamine Analysis in Pet Foods with High-Performance Liquid Chromatography with Diode Array Detection

机译:高效液相色谱-二极管阵列检测技术在宠物食品中三聚氰胺加压液体萃取中的适用性

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摘要

A pressurized liquid extraction (PLE) method was developed for melamine analysis in pet foods. The PLE method which utilized an accelerated solvent extraction (ASE®) system was also compared with sonication and polytron extraction methods. The parameters for the optimized PLE method were temperature (75 °C for wet pet food, 125 °C for dry pet food), pressure (1,500 psi), static time (10 min), flush volume (40%), purge time (1 min), and number of cycles (1). Recoveries obtained by PLE method were significantly higher (P ≤ 0.05) than those of sonication and polytron methods for dry pet food samples. For the analysis of adulterated pet foods, PLE resulted in the highest melamine content followed by sonication and polytron. Using PLE, samples fortified with melamine at 2.5 and 100 mg kg−1 resulted in recoveries ranging from 55% to 90% for wet samples and from 90% to 116% for dry samples. Low recovery rate from wet samples at low spike level (2.5 mg kg−1) may have been caused by co-aggregation of polysaccharide and protein with melamine due to low pH during solid-phase extraction cleanup. Limit of detection and limit of quantification values were 0.5 (mg kg−1) and 1.0 (mg kg−1) for dry samples. Overall, PLE had the best extraction efficiency compared to sonication and polytron, proving PLE to be a useful tool for melamine analysis of pet foods.
机译:开发了一种加压液体萃取(PLE)方法用于宠物食品中的三聚氰胺分析。使用加速溶剂萃取(ASE®)系统的PLE方法也已与超声和polytron萃取方法进行了比较。优化的PLE方法的参数为温度(湿宠物食品为75°C,干宠物食品为125°C),压力(1,500 psi),静态时间(10分钟),冲洗量(40%),吹扫时间( 1分钟),循环次数(1)。通过PLE方法获得的回收率显着高于(P≤0.05)干燥宠物食品样品的超声处理和polytron方法。对于掺假宠物食品的分析,PLE导致三聚氰胺含量最高,然后进行超声处理和polytron。使用PLE,以2.5和100 mg kg -1 的三聚氰胺强化的样品,湿样品的回收率在55%至90%之间,干样品的回收率在90%至116%之间。固相萃取净化过程中pH值较低,可能是由于多糖和蛋白质与三聚氰胺的共聚集所致,因此湿峰样品的回收率较低(2.5 mg kg -1 ),其回收率较低。干燥样品的检出限和定量限分别为0.5(mg kg -1 )和1.0(mg kg -1 )。总体而言,与超声和聚tron相比,PLE的提取效率最高,证明PLE是宠物食品中三聚氰胺分析的有用工具。

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