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在对健康有害的C18顺式/反式脂肪酸进行快速和常规气相色谱分析中使用双阳离子液体固定相的评估。

Evaluation of use of a dicationic liquid stationary phase in the fast and conventional gas chromatographic analysis of health-hazardous C18 cis/trans fatty acids.

作者信息

Ragonese Carla, Tranchida Peter Quinto, Dugo Paola, Dugo Giovanni, Sidisky Leonard M, Robillard Mark V, Mondello Luigi

机构信息

Dipartimento Farmaco-Chimico, Facoltà di Farmacia, Università dei Messina, Viale Annunziata, I-98168, Messina, Italy.

出版信息

Anal Chem. 2009 Jul 1;81(13):5561-8. doi: 10.1021/ac9007094.

Abstract

The present research is focused on the evaluation of one 0.10 mm i.d. and two 0.25 mm i.d., ionic liquid (IL) stationary phase [1,9-di(3-vinyl-imidazolium) nonane bis(trifluoromethyl) sulfonyl imidate] columns, with lengths of 12 (the microbore capillary), 30 and 100 m, in the GC analysis of cis/trans fatty acid methyl esters (FAMEs). The selectivity of the IL columns toward a series of standard C(18:1), C(18:2), and C(18:3) geometric isomers (a group of 22 compounds was subjected to GC analysis) was compared to the performance of a widely used column in the cis/trans FAMEs analysis field, viz., a 100 m x 0.25 mm i.d. capillary with a 0.20 microm stationary phase film of bis-cyanopropyl polysiloxane (SP-2560). The selectivity provided by the IL phase was superior if compared to that of the other well-established capillary. An optimized IL method, using the longer column, was subjected to validation: retention time and peak area intraday precision (n = 5) were good, with RSD values lower than 0.07% and 6.6%, respectively; LODs (considering a S/N of 3) for C(18:1Delta)(9tr) and C(18:2Delta)(9tr,12tr) were 0.15 (7.3 ppm) and 0.18 ng (9.1 ppm) on-column, respectively, while LOQs (considering a S/N of 10) were 0.49 (24.3 ppm) and 0.60 ng (30.2 ppm), respectively; the method was found to be linear, for both trans FAMEs, in the 10-2000 ppm range. For the evaluation of accuracy, a hydrogenated margarine, spiked with known amounts of C(18:3Delta)(9c,12c,15c), was subjected to analysis using C(13:0) as an internal standard.

摘要

本研究聚焦于内径为0.10 mm的一根色谱柱以及内径为0.25 mm的两根色谱柱,其固定相为离子液体(IL)[1,9 - 二(3 - 乙烯基 - 咪唑鎓)壬烷双(三氟甲基)磺酰亚胺],长度分别为12 m(微径毛细管柱)、30 m和100 m,用于顺式/反式脂肪酸甲酯(FAMEs)的气相色谱分析。将IL色谱柱对一系列标准C(18:1)、C(18:2)和C(18:3)几何异构体(一组22种化合物进行了气相色谱分析)的选择性与顺式/反式FAMEs分析领域广泛使用的一根色谱柱的性能进行了比较,即一根100 m×0.25 mm内径、固定相膜厚为0.20 µm的双氰丙基聚硅氧烷(SP - 2560)毛细管柱。与另一根成熟的毛细管柱相比,IL固定相提供的选择性更优。使用较长色谱柱的优化IL方法进行了验证:保留时间和峰面积日内精密度(n = 5)良好,相对标准偏差(RSD)值分别低于0.07%和6.6%;C(18:1Δ)(9tr)和C(18:2Δ)(9tr,12tr)的柱上检测限(考虑信噪比为3)分别为0.15 ng(7.3 ppm)和0.18 ng(9.1 ppm),而定量限(考虑信噪比为10)分别为0.49 ng(24.3 ppm)和0.60 ng(30.2 ppm);该方法对于两种反式FAMEs在10 - 2000 ppm范围内均呈线性。为评估准确度,使用C(13:0)作为内标对添加了已知量C(18:3Δ)(9c,12c,15c)的氢化人造黄油进行了分析。

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