CONDENSATION NUCLEATION LIGHT-SCATTERING DETECTION FOR CONVENTIONAL REVERSED-PHASE LIQUID-CHROMATOGRAPHY
CONDENSATION NUCLEATION LIGHT-SCATTERING DETECTION FOR CONVENTIONAL REVERSED-PHASE LIQUID-CHROMATOGRAPHY
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DOI：
10.1021/ac00099a026
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发表时间：
1995-02-01
影响因子：
7.4
通讯作者：
SZOSTEK, B
中科院分区：
文献类型：
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作者：
ALLEN, LB;KOROPCHAK, JA;SZOSTEK, B
本报告演示了冷凝成核光散射检测（CNLSD）与传统的反相液相色谱（RPLC）的接口。CNLSD是一种基于气溶胶的方法，其响应于溶剂蒸发后存在的颗粒的大小和数量。由于大多数HPLC级有机溶剂在蒸发后的残留物在微克/毫升范围内，因此发现溶剂纯度是一个限制。在本报告中，增加移动的相的有机物含量被证明会增加背景强度并阻碍灵敏度。还报道了两种减轻有机溶剂影响的方法。第一种方法涉及有机溶剂的化学纯化，第二种方法涉及通过去除较小尺寸的颗粒来改变最终或检测到的颗粒尺寸分布。后一种方法，使用扩散屏幕，被发现提供了4倍或更多的灵敏度增加，而不显着改变低分析物浓度的响应，与扩散屏幕不存在的情况下。报告了各种分析物的响应，结果显示几乎等同。对于典型的RPLC C18色谱柱，色谱柱流失不会限制性能。最后，通过比较对氨基苯磺酸和磺胺的分离性能，得到纳克级检测限的结果进行了总结。
This report demonstrates the interfacing of condensation nucleation light scattering detection (CNLSD) with conventional reversed-phase liquid chromatography (RPLC). CNLSD is an aerosol-based approach that responds to the size and number of particles present after solvent evaporation. As most HPLC grade organic solvents have listed residues after evaporation in the micrograms per milliliter range, solvent purity was found to be a limitation. In this report, increasing the organic content of the mobile phase is shown to increase the background intensity and hinder sensitivity. Two approaches to alleviating the influence of the organic solvent are also reported. The first approach involves the chemical purification of the organic solvent, and the second approach involves modifying the final or detected particle size distribution by removal of the smaller-sized particles. The latter approach, using diffusion screens, was found to provide an increase in sensitivity by a factor of 4 or more without significantly changing the response for low analyte concentrations, compared to the case where the diffusion screens were absent. Responses for various analytes are reported and shown to be nearly equivalent. For typical RPLC C18 columns, column bleed did not limit performance. Finally, results are summarized by comparing performance for the separation of sulfanilic acid and sulfanilamide, where nanogram level detection limits were obtained.