色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
6期
558-562
,共5页
吴顺%郝卫强%岳邦毅%张培培%狄斌%陈强
吳順%郝衛彊%嶽邦毅%張培培%狄斌%陳彊
오순%학위강%악방의%장배배%적빈%진강
液相色谱%梯度洗脱%梯度曲线%色谱峰宽
液相色譜%梯度洗脫%梯度麯線%色譜峰寬
액상색보%제도세탈%제도곡선%색보봉관
liquid chromatography%gradient elution%gradient profile%peak width
在梯度液相色谱中,溶剂混合以及轴向扩散等因素会使梯度曲线发生变形,而这在阶梯梯度以及高斜率的线性梯度中表现得尤为明显。本文探讨了这种梯度曲线变形对色谱峰宽的影响。首先以 C18色谱柱为固定相,甲醇-水为流动相,联苯和苯乙酮为样品,测得不同线性梯度和阶梯梯度条件下的色谱峰。然后以205 nm 为检测波长,记录相应条件下未接色谱柱时甲醇的响应值,得到柱入口处的梯度曲线。接着根据所设定的梯度条件以及柱入口处测得的梯度曲线,分别计算相应情形中色谱峰宽的理论值,将其与实验值进行了比较。研究结果表明,梯度曲线的变形会对色谱峰宽产生影响。当将这种影响考虑在内后,理论值与实验值更为吻合。
在梯度液相色譜中,溶劑混閤以及軸嚮擴散等因素會使梯度麯線髮生變形,而這在階梯梯度以及高斜率的線性梯度中錶現得尤為明顯。本文探討瞭這種梯度麯線變形對色譜峰寬的影響。首先以 C18色譜柱為固定相,甲醇-水為流動相,聯苯和苯乙酮為樣品,測得不同線性梯度和階梯梯度條件下的色譜峰。然後以205 nm 為檢測波長,記錄相應條件下未接色譜柱時甲醇的響應值,得到柱入口處的梯度麯線。接著根據所設定的梯度條件以及柱入口處測得的梯度麯線,分彆計算相應情形中色譜峰寬的理論值,將其與實驗值進行瞭比較。研究結果錶明,梯度麯線的變形會對色譜峰寬產生影響。噹將這種影響攷慮在內後,理論值與實驗值更為吻閤。
재제도액상색보중,용제혼합이급축향확산등인소회사제도곡선발생변형,이저재계제제도이급고사솔적선성제도중표현득우위명현。본문탐토료저충제도곡선변형대색보봉관적영향。수선이 C18색보주위고정상,갑순-수위류동상,련분화분을동위양품,측득불동선성제도화계제제도조건하적색보봉。연후이205 nm 위검측파장,기록상응조건하미접색보주시갑순적향응치,득도주입구처적제도곡선。접착근거소설정적제도조건이급주입구처측득적제도곡선,분별계산상응정형중색보봉관적이론치,장기여실험치진행료비교。연구결과표명,제도곡선적변형회대색보봉관산생영향。당장저충영향고필재내후,이론치여실험치경위문합。
In gradient liquid chromatography,the gradient profile may be distorted because of the effects of solvent mixing and axial dispersion. Such effects will be significant especially when stepwise gradient and linear gradient with high slope are applied. In this work,we dis-cussed the influence of the distortion of gradient profile on the peak width. Firstly,the chroma-tographic peaks were measured under linear and stepwise gradient conditions where a C18 col-umn was used as the stationary phase,a mixture of methanol and water as the mobile phase, and biphenyl and acetophenone as the samples. Then,the response of methanol under corre-sponding conditions was recorded by disconnecting the column and the detection wavelength was set at 205 nm. The gradient profile at the column inlet was calculated from the methanol response profile. The theoretical values of the peak width were calculated from the set gradient profile and the gradient profile obtained at the column inlet respectively. The theoretical values were compared with the experimental ones. It is shown that the distortion of gradient profile does affect the peak width. When such influence is taken into account,the theoretical and experimental values of the peak width are well consistent.