Determination of illegal added rosiglitazone in dietary supplement by multi-walled carbon nanotubes dispersive solid-phase extraction combined with high performance liquid chromatography
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摘要: 本文建立多壁碳纳米管分散型固相萃取-高效液相色谱法测定降糖类保健食品中非法添加物罗格列酮的检测方法,重点考察了样品提取溶剂和提取时间、净化剂类型、组成、使用量和净化时间对回收率的影响。结果表明,样品前处理最优条件为:采用无水甲醇超声提取20 min,经多壁碳纳米管（MWCNTs）和N-丙基乙二胺（PSA）净化1 min。所建立的高效液相色谱法测定降糖类保健食品中罗格列酮的线性范围为1.050.0μg/m L,相关系数为0.9997,检出限和定量限分别是0.02μg/m L和0.06μg/m L。样品加标平均回收率为77.3%93.2%,相对标准偏差（RSD）小于10%。该样品前处理方法简便、快速且成本较低,适用于批量保健食品中罗格列酮的快速检测。Abstract: With the aim of developing an optimal sample pretreatment for the determination of illegal added rosiglitazone in dietary supplement,a method was developed using carbon nanotubes dispersive solid- phase extraction combined with high performance liquid chromatography( HPLC). Key parameters that affect impurity removal and recovery of samples were optimized including the sample extraction solvent and extraction time,the type,composition,amount of purifying agent and sample purifying time. The optimal sample pretreatment conditions were achieved as follows: samples were ultrasonically extracted for 20 min using absolute methanol,and.then cleaned up for 1 min with multi- walled carbon nanotubes( MWCNTs)and N- propyl ethylenediamine( PSA) before analysis. The HPLC method established based on the optimized sample pretreatment conditions exhibited a good linear relationship from 1.0 to 50.0 μg / m L,with the correlation coefficient of 0.9997.The limit of detection and quantification was 0.02 and 0.06 μg / m L,respectively.The mean spike recovery rates for rosiglitazone in dietary supplement were in the range of 77.3% ~93.2%,with relative standard deviations( RSD) less than 10%. This method was simple,rapid,low- cost and applicable for the determination of illegal added drug rosiglitazone in dietary supplement.
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