主题:谁能提供下HPLC检测器相关资料

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hardlystop
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有人有HPLC检测器的分类及相关的相应机理,ELSD的相应原理是什么?谁有这方面的资料?
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36violet
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36violet
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hardlystop
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原文由 36violet 发表:
我传上了啊!怎么会没有呢?

没见到,在传一次。
我在故我思
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原文由 hardlystop 发表:
有人有HPLC检测器的分类及相关的相应机理,ELSD的相应原理是什么?谁有这方面的资料?

The Evaporative Light Scattering Detector
The evaporative light scattering detector, as its name implies, utilizes  a spray that continuously atomizes the column eluent into small droplets. These droplets are allowed to evaporate, leaving the solutes as fine particulate matter suspended in the atomizing gas.

The atomizing gas can be air or, if necessary, an inert gas. The suspended particles pass through a light beam and the scattered light viewed at 45o to the incident light beam by means of a pair of optical fibers. The scattered light transmitted through the fibers is sensed by a photomultiplier and the output electronically processed and passed either to a computer data acquisition system or to a potentiometric recorder. A diagram of the light scattering detector is shown in figure 48. Theoretically, the detector responds to all solutes that are not volatile and as the light dispersion is largely Raleigh scattering, the response should be proportional to the mass of solute present; as a consequence, it is sometimes referred to as the mass detector. For a linear response, the droplet size must be carefully controlled as it also determines the particle size of the dried solutes.
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Detector sensitivity is claimed to be between 10 and 20 ng of solute. However, in these terms it is difficult to compare with other detectors. The great advantage of the detector, however, is its catholic response and that its output is linearly related to the mass of solute present. However, the magnitude of the response does vary widely between different substances.

A diagram of the sensor of the evaporative light scattering detector manufactured by Polymer Laboratories is shown in figure 49. The eluent is atomized in a stream of nitrogen and the finely divided spray passes down a heated chamber during which time the solvent is evaporated. The removal of the solvent produces a stream of particles which then pass through a collimated beam of light. The scattered light at an angle to the incident light is focused onto a photomultiplier tube and the output is processed in an appropriate manner electronically.
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ELSD的原理极简单。HPLC柱分离后的洗脱液使用喷雾器在干空气中喷雾加温时,从洗脱液的雾中溶剂蒸发,析出溶解的溶质分子。这个粒子进行光散射检测。(只洗脱液时,全量蒸发成为无检测状态)。

初期的ELSD使用洗脱液雾的全量蒸发系统。由于洗提液雾不是均匀的粒径,大粒径的液滴较难蒸发,这是产生噪声的原因。

巧妙的清除方法,是法国SEDERE公司开发的ELSD。洗脱液雾在玻璃管中喷雾,大粒径的雾由于重力自由降落除去。只有通过玻璃管的细雾导入加温管,进入光散射检测器。这样简单而伟大的创举,促使ELSD取得飞跃的进步。以下是ELSD的特征。

ELSD的优点
·不挥发的物质可检测
·由于溶剂蒸发,即使进行梯度法也不会影响基线。
·受外部温度的影响少

ELSD的缺点
·只能使用挥发性洗脱液(碳酸铵盐:所谓LC-MS洗脱液)
·挥发性物质检测灵敏度非常低
·与UV相比,检测灵敏度小,动态量程小
·可以检测到多余的物质(柱流失物)

ELSD的运用范围
上述的ELSD不是万能的。因此,期待能成为UV检测器的补充。
药物杂质分析是件「保险」的事。立脚于「也许有杂质」上的位置,使用多方面的检测手段进行保险。它的保险之一是ELSD。
除使用ELSD探索杂质外,化合物若是特定的话,也可使用灵敏度高的衍生化法。

ELSD的灵敏度提高
ELSD与UV比较虽然检测灵敏度较低,但我公司找到了提高灵敏度的对策。那是称为LC-MS用离子对试剂的氟羧酸。最初的目的是,采用离子对为了增加柱的保留效果,却意外地发现大幅度地提高灵敏度。分析对象是挥发性高的物质时,ELSD灵敏度几乎没有,但是,①由于与氟羧酸的离子对加合,分子量增加降低了挥发性,②由于离子对形成阻碍了柱的吸附。
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hezy129
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资料中心有,论坛上搜索一下,至少有示差检测器(本人上传)ELSD,这些都有,如果没有或找不到,大家可以和我联系,我们定个贴区专门传一下,留言周六日上传即可
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