首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >The determination of patulin from food samples using dual-dummy molecularly imprinted solid-phase extraction coupled with LC-MS/MS
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The determination of patulin from food samples using dual-dummy molecularly imprinted solid-phase extraction coupled with LC-MS/MS

机译:使用双伪分子印迹固相萃取与LC-MS / MS的双伪分子印迹固相萃取测定食品样品的鉴定

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摘要

A molecularly imprinted polymer (MIP) with specific adsorption for patulin was successfully polymerized by precipitation polymerization using 2-oxindole (2-oxin) and 6-hydroxynicotinic acid (6-HNA) as dummy template molecules, methylacrylic acid (MAA) as a functional monomer, trimethylolpropane trimethacrylate (TRIM) as a crosslinker, 2,2-azobis-(2-methylpropionitrile) (AIBN) as a initiator, and methanol as a porogen solvent. The molecularly imprinted solid phase extraction (MI-SPE) column was prepared using the polymer as a sorbent and applied for the selective extraction of patulin from real samples. The results showed that the MI-SPE method had high selectivity and specific adsorption towards patulin with mean recoveries ranged between 81.3% and 106.3% and a relative standard deviation (RSD) < 4.5%. Additionally, the developed MI-SPE method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) exhibited good linearity in the range of 1-100 ng mL(-1) with correlation coefficients (R-2) > 0.998. The limits of detection (LODs, S/N = 3) were 0.05-0.2 ng g(-1), and the limits of quantification (LOQs, S/N = 10) were 0.2-0.5 ng g(-1). The developed method showed a better purification and higher patulin recovery for real samples than the quick, easy, cheap, effective, rugged, safe "QuEChERS" method.
机译:通过使用2-氧吲哚(2- X X键)和6-羟基肉酸(6-HID)作为假模板分子,甲基丙烯酸(MAA)作为函数的沉淀聚合,通过沉淀聚合成功地聚合具有特异性吸附的分子印迹聚合物(MIP)。单体,三羟甲基丙烷三甲基丙烯酸酯(修剪)作为交联剂,2,2-偶氮二硝基甲腈)(A-甲基丙腈)(AIBN)作为引发剂,以及甲醇作为致致孔溶剂。使用聚合物作为吸附剂制备分子印迹固相萃取(MI-SPE)柱,并施加来自真实样品的髌粉的选择性提取。结果表明,MI-SPE方法具有高选择性和对鉴定的特异性吸附,平均回收率范围为81.3%和106.3%,相对标准偏差(RSD)<4.5%。另外,与液相色谱 - 串联质谱(LC-MS / MS)耦合的开发的MI-SPE方法在1-100ng mL(-1)的范围内具有相关系数(R-2)> 0.998的良好线性。检测限(LODS,S / N = 3)为0.05-0.2ng(-1),并且量化的限制(LOQs,S / N = 10)为0.2-0.5ng g(-1)。该方法显示出比快速,简单,便宜,有效,安全的“QueCher”方法更好地纯化和更高的鉴定性净化和更高的鉴定性恢复。

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