On-line enrichment-substep focus sample introduction-ultra-high performance liquid chromatography combination system and application

An ultra-high-efficiency liquid phase and sample injection technology, which is applied in the field of analytical chemical sample pretreatment, can solve problems such as deformation and eluent volume overload, and achieve the effects of expanding the selection range, avoiding peak broadening and deformation, and improving sensitivity

Active Publication Date: 2013-06-05
SUN YAT SEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve the problem that the online enrichment eluent easily causes the broadening and deformation of the ultra-high performance liquid chromatography peak, and designs an online enrichment-step-by-step focusing sampling-ultra-high performance liquid chromatography combined system. The strategy of step-by-step focus solves the problem of eluent volume overload, realizes the online combination of enrichment technology and ultra-high performance liquid chromatography, relaxes the limitation of UHPLC on the pressure resistance performance of extraction materials and the volume of extraction phase, and improves the resolution and analysis efficiency and sensitivity

Method used

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  • On-line enrichment-substep focus sample introduction-ultra-high performance liquid chromatography combination system and application
  • On-line enrichment-substep focus sample introduction-ultra-high performance liquid chromatography combination system and application
  • On-line enrichment-substep focus sample introduction-ultra-high performance liquid chromatography combination system and application

Examples

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Effect test

Embodiment 1

[0056] Example 1: Analysis of triazine herbicides in water samples using an online enrichment-step focused sampling-ultra-high performance liquid chromatography system.

[0057] Experimental drugs, instruments and conditions: the samples were spiked tap water of 8 kinds of triazine herbicides, using ultra-high performance liquid chromatography and C18 reversed-phase chromatographic column (specification 3.0×100mm, particle size 2.2μm), the initial mobile phase was 5% acetonitrile, hold for 0.5min after injection, then increase to 38% within 11.5min, and finally increase to 100% for 3min; flow rate 1mL / min, extraction column (Inertsil ODS-SP column, 4.0×10.0mm, 5μm) .

[0058] On-line enrichment-step focused sampling-ultra-high performance liquid chromatography combined system such as figure 1 As shown, the operation steps and the positions of the corresponding valves are shown in Table 1. The specific operation of each step is as follows: 1) 4mL tap water sample is injected i...

Embodiment 2

[0062] Example 2: Analysis of six pollutants containing benzene rings by ultra-high performance liquid chromatography with step-by-step focused large-volume injection method.

[0063] Experimental drugs, instruments and conditions: the sample is an acetonitrile solution containing nitrobenzene, toluene, o-dichlorobenzene, butyl phthalate, benzofluoranthene and octyl phthalate, and the ultra-high performance liquid chromatography is used to And C18 reverse-phase chromatographic column (specification 3.0×100mm, particle size 2.2μm), using high-pressure six-way injection valve, 1mL stainless steel quantitative loop to achieve multi-step focused sampling, the initial mobile phase is 5% acetonitrile, and the flow rate is 1mL / min.

[0064] The ultra-high performance liquid chromatography step-focused large-volume sampling device is a simplification of the online enrichment-step focus sampling-ultra-high performance liquid chromatography combined system, such as figure 1 As shown in ...

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Abstract

The invention discloses a substep focus sample introduction-ultra-high performance liquid chromatography combination system and a combination method thereof and an on-line enrichment-substep focus sample introduction-ultra-high performance liquid chromatography combination system and a combination method thereof. The enrichment-substep focus sample introduction-ultra-high performance liquid chromatography combination system comprises on-line enrichment devices, a substep focus sample introduction device and an ultra-high performance liquid chromatography device, wherein every two on-line enrichment devices are connected mutually. The problems that the overloaded volume of the ultra-high performance liquid chromatography is caused by eluant can be solved through a strategy of the substep focus sample introduction. An on-line combination analysis of an enrichment method and the ultra-high performance liquid chromatography can be achieved. Under the premise of obtaining sharpened bands, the on-line enrichment and a rapid separating analysis can be carried out, and analytical sensitivity, speeds and automation degrees can be improved.

Description

technical field [0001] The invention belongs to the field of analytical chemical sample pretreatment, and specifically relates to the design, analysis and application of an online enrichment-step-by-step focusing sampling-ultra-high performance liquid chromatography system, which is suitable for complex applications such as environment, food, medicine, and biology. On-line pretreatment, extraction, desorption, separation and detection of trace organics in samples. Background technique [0002] Ultra High Performance Liquid Chromatography (UHPLC) is a powerful analytical tool for its fast separations and high sensitivity. However, when applied to ultra-trace analysis of complex samples, efficient pre-treatment techniques are usually required for purification and enrichment, such as solid phase extraction (SPE) and solid phase microextraction (SPME). At present, the enrichment technology and UHPLC are usually used in an off-line manner. This is because the UHPLC column is sho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 李攻科潘加亮胡玉玲
Owner SUN YAT SEN UNIV
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