WO2007095794A1 - Dispositif d'électrochromatographie capillaire haute pression multifonctions - Google Patents

Dispositif d'électrochromatographie capillaire haute pression multifonctions Download PDF

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Publication number
WO2007095794A1
WO2007095794A1 PCT/CN2006/002480 CN2006002480W WO2007095794A1 WO 2007095794 A1 WO2007095794 A1 WO 2007095794A1 CN 2006002480 W CN2006002480 W CN 2006002480W WO 2007095794 A1 WO2007095794 A1 WO 2007095794A1
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capillary
column
purpose pressurized
capillary column
detector
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PCT/CN2006/002480
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English (en)
French (fr)
Inventor
Chao Yan
Xiaojing Huang
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Unimicro (Shanghai) Technologies Co., Ltd.
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Publication of WO2007095794A1 publication Critical patent/WO2007095794A1/zh

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416—Systems
    • G01N27/447—Systems using electrophoresis
    • G01N27/44756—Apparatus specially adapted therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/16—Injection
    • G01N30/20—Injection using a sampling valve

Definitions

  • Multi-purpose pressurized capillary electrochromatography device Multi-purpose pressurized capillary electrochromatography device
  • the present invention relates to an electrochromatographic separation detecting apparatus, and more particularly to a multi-purpose pressurized capillary electrochromatographic apparatus.
  • chromatographic separation detection devices are mostly composed of a driving device, a separation medium (column or capillary), and a detection device.
  • the gas chromatograph device consists of a gas source, a gas chromatographic column and a detection device. It is mainly used to separate gas mixtures and substances with low boiling point and easy gasification.
  • the liquid chromatography equipment by high pressure pump. The liquid chromatography column and the detection equipment are mainly used for separating the liquid mixture. The separation selectivity is good and the application range is wide.
  • the third is a capillary electrophoresis device, which is composed of a high-voltage power source, a quartz capillary tube and a detecting device.
  • the driving force is an electroosmotic flow, and the mobile phase moves forward in a capillary tube with a small diffusion, so that it can be obtained.
  • capillary electrochromatography device consisting of high-voltage power supply, capillary column with packing and detection equipment, this device has high choice of liquid phase Sexual, and has a high efficiency of capillary electrophoresis, but in the practical process, bubbles are generated to interrupt the current, resulting in failure to obtain Set, high precision analysis results, and since it does not have a gradient functions, thereby reducing their ability to handle complex actual samples.
  • Dr. Yu Chao one of the inventors of the present application, invented a multi-purpose pressurized electrochromatography device (Chinese patent)
  • a high-pressure pump is added to the capillary electrochromatography device, and the generation of bubbles is suppressed by pressurizing the capillary column, and high selectivity and high efficiency can be maintained.
  • the device has a strong analytical capability for practical complex samples by performing functions such as gradient elution. At the same time, the accuracy and reproducibility of the analysis are ensured by the use of a quantitative valve injection in the device.
  • the device uses a precision one-way valve Good results are achieved for components that separate the flow phase and control the pressure.
  • a simpler shunting method is used to obtain a stable nano-upgrade and micro-upgrade flow rate from a conventional high-pressure pump, and at the same time, the pressure delivery system, the injection valve and the shunt are isolated from the high-voltage electric field by an electrical isolating device, and The volume of the analytical sample can be flexibly changed.
  • the technical problem to be solved by the present invention is to provide a multi-purpose pressurized capillary electrochromatography device, in particular to a multi-purpose pressurized capillary electrochromatography device with stable performance, high analytical precision, and variable sample volume entering a capillary column. .
  • the present invention relates to a multi-purpose pressurized capillary electrochromatography apparatus comprising a high-pressure pump, a mixing valve, an injection valve, a capillary column, a detector, and a high-voltage power supply for supplying a voltage to a capillary column.
  • the utility model further comprises a shunt, one end is connected to the injection valve; an electric isolation device is connected at one end to the shunt and the other end is connected to the capillary column and the detector.
  • the invention adopts the above technology, has extremely high analysis precision, ensures the accuracy of the analysis result, and can adopt a shunting method for the sample, controls the volume of the sample volume, increases the flexibility of the system, and promotes the analysis method.
  • the establishment and optimization has a very good effect.
  • FIG. 1 is a structural view of a multi-purpose pressurized capillary electrochromatography apparatus of the present invention
  • FIG. 2 is an electric chromatogram of separating a sample of aniline and benzoic acid by using a multi-purpose pressurized capillary electrochromatography apparatus of the present invention
  • Figure 3 is an electrical chromatogram of the separation of ink samples using the multi-purpose pressurized capillary electrochromatography apparatus of the present invention. Best practice
  • the multi-purpose pressurized capillary electrochromatography apparatus of the present invention is shown in Fig. 1, and the suction end of the high pressure pump 3 is sucked.
  • the tube 2 is passed into the mobile phase 1 and its output is connected to the mixing valve 4.
  • the mixing valve 4 is connected to the splitter 6 or the injection valve 7 through a connecting pipe and enters the separation system 10.
  • the mobile phase 1 pushes the sample through the injection valve and then splits into the separation capillary or directly into the separation capillary without splitting.
  • the splitter 6 consists of one or more capillary columns that control the pressure of the system by varying the length of the column, the diameter of the tube, and the size of the channel formed by the packing in the column.
  • the capillary separation system is stable to nano-upgrade.
  • the splitter 6 finely shunts the mobile phase and the sample.
  • the on-off valve 11 and the current limiting device 12 are connected to the flow divider 6, which can more flexibly adjust the split ratio and facilitate operation.
  • the sample after being split by the splitter 6 is passed through the connecting tube into the capillary separation system.
  • the capillary separation system employs an electrical isolation device 5 which functions to isolate the high pressure pump 3, the mixing valve 4, the injection valve 7 and the splitter 6 from the high voltage electric field.
  • the electrical isolation device 5 ensures that the solution flowing out of the flow divider 6 smoothly flows into the separation capillary column 8 without flowing into the electrical isolation device 5 while ensuring the closed loop of the electric field.
  • the electric isolator 5 can be made of porous glass, porous graphite, Naf ion ion exchange membrane, cellulose acetate, metal palladium, sintered glass, etched quartz, glass, and the like.
  • the high voltage power source 15 applies an electric field across the separation capillary column 8 by connecting the electrode 14 at the electrical isolation device 5 and the wire separating the electrode 14 at the end of the capillary column 8, to achieve dual drive of the electric field and pressure to the mobile phase and the sample.
  • the rear window of the separation capillary column 8 is opposed to the optical path of the detector 9, and the detector 9 is connected to a computer.
  • the sample finally passed through the detector 9 flows into the waste liquid pool 16 through a connecting pipe through a four-way valve 13 provided at the end of the separation capillary column 8.
  • This example uses the present invention to separate a sample of aniline and benzoic acid.
  • the capillary column with packing was taken as a capillary separation system, and the sample was analyzed by high-voltage power supply and high-pressure pump drive.
  • the device has a dual separation mechanism with a multi-purpose pressurized electrochromatograph that adjusts the voltage and mobile phase gradient to improve resolution.
  • a very high analytical method is obtained by using the device of the invention Method flexibility and analytical accuracy.
  • the C18 packed capillary column with an inner diameter of 150 ⁇ ⁇ , an effective column length of 30 cm, a total length of 50 cm and a particle size of 5 ⁇ m was used to separate the aniline and benzoic acid mixed samples by pressure electrochromatography.
  • the mobile phase was methanol: water 70: 30 (containing 5 mmol/l phosphate buffer).
  • the detection wavelength is 254 nm, the voltage is -10 kV, and the pressure is 8. 5 MPa.
  • This example applies the present invention to separate ink samples.
  • the ink sample was separated by pressure electrochromatography using a C18 packed capillary column with an inner diameter of 150 ⁇ m, an effective column length of 30 cm, a total length of 50 cm, and a particle size of 5 ⁇ m.
  • the mobile phase is A: 5% acetonitrile + 95% water + 0. 05% TFA, B: 100% acetonitrile + 0. 05% TFA.
  • Detection wavelength 214nm, voltage - 10kV, pressure 9. 4MPa D
  • each peak retention time RSD (%) is within 1%
  • the peak retention time RSD (%) of each peak area is at most 2.5%
  • the analysis accuracy of complex samples is guaranteed ( Figure 3 Show). Thereby the sample is carefully separated.

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  • Physics & Mathematics (AREA)
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Description

多用加压毛细管电色谱装置 技术领域
本发明涉及一种电色谱分离检测装置， 尤其涉及一种多用加压毛细管电色 谱装置。
背景技术
目前， 色谱分离检测装置多由驱动装置、 分离介质 （色谱柱或毛细管） 以 及检测设备构成。 主要有以下几种： 一是气相色谱装置， 由气源、 气相色谱柱 和检测设备构成， 主要用于分离气体混合物和沸点低、 易气化的物质； 二是液 相色谱装置， 由高压泵、 液相色谱柱和检测设备构成， 主要用于分离液态混合 物， 分离选择性好， 应用范围广， 但由于驱动力是压力， 流动相在固定相上呈 抛物线式前移， 有扩散， 因而柱效较低； 三是毛细管电泳装置， 由高压电源、 石英毛细空管和检测设备构成， 其特点是驱动力是电渗流， 流动相在毛细管内 呈柱塞式前移， 扩散小， 因而可以获得良好的柱效， 但对中性样品 （不带电） 选择性不好； 四是毛细管电色谱装置， 由高压电源、 带填料的毛细管柱和检测 设备构成， 这种装置既具有液相的高选择性， 又具有毛细管电泳的高柱效， 但 实用过程中易产生气泡使电流中断， 导致无法获得稳定、 高精度的分析结果， 同时， 由于其不具备梯度洗脱等功能， 从而降低了其处理实际复杂样品的能力。
本申请的发明人之一阎超博士曾发明了多用加压电色谱装置 （中国专利
CN2373793Y), 在毛细管电色谱装置的基础上增加了高压泵， 通过对毛细管色谱 柱加压抑制气泡的产生， 并能保持高选择性和高柱效。 该装置通过实施梯度洗 脱等功能， 具有对实际复杂样品很强的分析能力。 同时， 该装置中由于采用了 定量阀进样， 保证了分析的准确性和重现性。 该装置中采用了精密的单向阀作 为流动相分流和控制压力的元件， 取得较好效果。
本发明中釆用了更简单的分流方法， 从常规的高压泵获得稳定的纳升级和 微升级流速， 同时， 通过电隔离装置将压力输送系统、 进样阀和分流器与高压 电场隔离， 并可灵活改变分析样品的体积。
发明内容
本发明要解决的技术问题是提供一种多用加压毛细管电色谱装置， 尤其涉 及一种性能稳定、 具有极高分析精度、 并且可改变进入毛细管色谱柱中样品体 积的多用加压毛细管电色谱装置。
为解决上述技术问题， 本发明一种多用加压毛细管电色谱装置， 其由顺序 连接的高压泵、 混合阀、 进样阀、 毛细管色谱柱、 检测器及对毛细管色谱柱提 供电压的高压电源组成， 更包含有一分流器， 一端与进样阀相连； 一电隔离装 置， 一端与所述分流器相连， 另一端与毛细管色谱柱和检测器相连。
本发明由于采用了上述技术， 具有极高的分析精度， 保证了分析结果的准 确性， 并可对样品采用分流的方式， 控制分析样品量的体积， 增加了系统的灵 活性， 对促进分析方法的建立和优化具有很好的效果。
附图说明
图 1是本发明一种多用加压毛细管电色谱装置的结构图；
图 2是应用本发明多用加压毛细管电色谱装置分离苯胺、 苯甲酸混合样品 的电色谱图；
图 3是应用本发明多用加压毛细管电色谱装置分离油墨样品的电色谱图。 最佳实施方式
下面结合附图及实施例对本发明作进一步详细的说明。
本发明多用加压毛细管电色谱装置如图 1所示， 高压泵 3的吸入端通过吸 管 2通入流动相 1中， 其输出端与混合阀 4相连。 混合阀 4通过连接管与分流 器 6或进样阀 7相连， 进入分离体系 10。 流动相 1推动样品可先通过进样阀 Ί 再分流后进入分离毛细管， 也可不分流直接进入分离毛细管。 分流器 6 由一根 或多根毛细管柱组成， 这些毛细管柱通过改变柱长度、 管径， 以及柱内的填充 物形成的通道尺寸来控制系统的压力， 毛细管分离体系稳定的纳升到微升级的 流速和分流比。 通过这种方式， 分流器 6对流动相与样品进行细致分流。 开关 阀 11和限流装置 12与分流器 6相连， 可更灵活调节分流比， 方便操作。 经过 分流器 6分流后的样品沿连接管通入毛细管分离体系中。 毛细管分离体系采用 了电隔离装置 5， 该装置的作用是将高压泵 3、 混合阀 4、 进样阀 7以及分流器 6与高压电场隔离。该电隔离装置 5在保证电场闭合回路的同时，保证由分流器 6流出的溶液顺利流入分离毛细管色谱柱 8， 而不流入到电隔离装置 5中。 该电 隔离装置 5可以采用多孔玻璃类， 多孔石墨类， Naf ion离子交换膜类， 醋酸纤 维素类， 金属钯类， 烧结玻璃类以及蚀刻石英、 玻璃类等。 高压电源 15通过连 接电隔离装置 5处的电极 14和分离毛细管色谱柱 8尾端的电极 14的导线在分 离毛细管色谱柱 8两端施加电场， 实现电场和压力对流动相和样品的双重驱动。 分离毛细管色谱柱 8后部窗口与检测器 9的光路相对， 检测器 9与计算机相连。 最终经过检测器 9的样品通过设置在分离毛细管色谱柱 8末端的四通阀 13经连 接管流入废液池 16。
实施例 1
本实施例应用本发明分离苯胺、 苯甲酸混合样品。
取带填料的毛细管色谱柱作为毛细管分离体系， 同时采用高压电源和高压 泵驱动， 对样品进行分析。 该装置具有多用加压电色谱仪的双重分离机制， 可 调节电压和流动相梯度来改善分离度。 采用本发明中装置获得了极高的分析方 法的灵活性和分析精度。
釆用内径 150 μ πι， 有效柱长 30cm， 总长 50cm ， 5 μ m粒径的 C18填料毛细 管柱， 以加压电色谱法分离苯胺、 苯甲酸混合样品。 流动相为甲醇： 水 70: 30 (含 5mmol/l磷酸盐缓冲溶液）。 检测波长 254nm， 加电压 - 10kV， 压力 8. 5MPa。
重复实验 7次， 出峰时间和峰面积的 RSD (%)均在 1%以内 （如图 2所示）。 从 而将样品细致分离。
实施例 2
本实施例应用本发明分离油墨样品。
采用内径 150 μ πι, 有效柱长 30cm， 总长 50cm ， 5 μ m粒径的 C18填料毛细 管柱， 以加压电色谱法分离油墨样品。采用梯度洗脱， 流动相为 A: 5%乙腈 +95% 水 +0. 05%TFA ， B: 100%乙腈 +0. 05%TFA。 检测波长： 214nm, 加电压 - 10kV， 压 力 9. 4MPaD
重复进样 5次， 各峰保留时间 RSD (%)均在 1%以内， 各峰峰面积的保留时 间 RSD (%)最大在 2. 5%， 复杂样品的分析精度得到保障（如图 3所示）。 从而 将样品细致分离。

Claims

权利要求
1、 一种多用加压毛细管电色谱装置， 其由顺序连接的高压泵、 混合阀、 进 样阀、 毛细管色谱柱、 检测器及对毛细管色谱柱提供电压的高压电源组成， 其 特征在于， 更包含： 一分流器， 一端与进样阀相连； 一电隔离装置， 一端与所 述分流器相连， 另一端与毛细管色谱柱和检测器相连。
2、 根据权利要求 i所述的多用加压毛细管电色谱装置， 其特征在于： 所述 分流器可以有一个、 两个甚至更多的出口。
3、 根据权利要求 1所述的多用加压毛细管电色谱装置， 其特征在于： 所述 分流器由一根、 或多根毛细管柱组成。
4、 根据权利要求 1所述的多用加压毛细管电色谱装置， 其特征在于： 所述 毛细管色谱柱可以是有填充物， 也可以是空管（即为毛细管电泳装置）。
5、 根据权利要求 3所述的多用加压毛细管电色谱装置， 其特征在于： 所述 毛细管柱材料可以是石英、 玻璃、 陶瓷， 也可以是聚合物等。
6、 根据权利要求 3所述的多用加压毛细管电色谱装置， 其特征在于： 所述 分流器毛细管柱可以是有填充物， 也可以是空管。
7、 根据权利要求 1所述的多用加压毛细管电色谱装置， 其特征在于： 所述 电隔离装置可以是多孔玻璃类， 多孔石墨类， Nafion离子交换膜类， 醋酸纤维 素类， 金属钯类， 烧结玻璃类以及蚀刻石英、 玻璃类等。
PCT/CN2006/002480 2006-02-23 2006-09-21 Dispositif d'électrochromatographie capillaire haute pression multifonctions WO2007095794A1 (fr)

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CN106680404A (zh) * 2017-02-22 2017-05-17 厦门色谱分析仪器有限公司 基于微流控芯片的液相色谱分流装置
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CN103884814B (zh) * 2014-04-17 2015-10-14 厦门大学 万伏高压电场增强液相色谱系统
CN104502472B (zh) * 2014-12-05 2016-06-01 上海交通大学 加压制备型电色谱在线检测与样品收集用电安全保护装置
CN104614457B (zh) * 2015-01-13 2016-08-17 上海交通大学 一套中压制备型电色谱分离装置
CN107037161A (zh) * 2017-06-13 2017-08-11 厦门大学 一种虹吸式毛细管色谱分离法

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CN106680404A (zh) * 2017-02-22 2017-05-17 厦门色谱分析仪器有限公司 基于微流控芯片的液相色谱分流装置
CN106680404B (zh) * 2017-02-22 2022-08-23 厦门色谱分析仪器有限公司 基于微流控芯片的液相色谱分流装置
CN106840825A (zh) * 2017-03-01 2017-06-13 上海通微分析技术有限公司 一种电隔离装置及其制作方法

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