CN103972020A - Analytical method for ion mobility spectrometry - Google Patents
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- 238000004458 analytical method Methods 0.000 title claims abstract description 13
- 238000001871 ion mobility spectroscopy Methods 0.000 title claims description 22
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 38
- 230000005012 migration Effects 0.000 claims abstract description 22
- 238000013508 migration Methods 0.000 claims abstract description 22
- 239000007789 gas Substances 0.000 claims description 64
- 239000012159 carrier gas Substances 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 abstract description 84
- 229910052717 sulfur Inorganic materials 0.000 abstract description 10
- 239000011593 sulfur Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 5
- 238000001228 spectrum Methods 0.000 abstract description 5
- 230000002452 interceptive effect Effects 0.000 abstract description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 30
- -1 oxygen ion Chemical class 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 230000005684 electric field Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012491 analyte Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002903 organophosphorus compounds Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种离子迁移谱的分析方法。在离子迁移管的电离反应区和迁移区之间设置一个离子消耗区。离子消耗区内含有特定的有机试剂分子，可以选择性地消除干扰离子，不仅提高了目标离子的分离度，而且避免了对电离反应区和迁移区的影响。本发明论述了该方法在检测硫磺中的应用。The invention discloses an analysis method of ion mobility spectrum. An ion consumption zone is set between the ionization reaction zone and the migration zone of the ion transfer tube. The ion depletion area contains specific organic reagent molecules, which can selectively eliminate interfering ions, which not only improves the separation of target ions, but also avoids the impact on the ionization reaction area and migration area. The invention discusses the application of the method in detecting sulfur.
Description
技术领域technical field
本发明涉及了一种离子迁移谱分析方法。以离子迁移谱为技术支持，在离子迁移管的电离反应区和迁移区之间设置一个离子消耗区，用于选择性地消除干扰离子，提高分离度的同时不影响电离反应区内的分子-离子反应。The invention relates to an ion mobility spectrum analysis method. With the technical support of ion mobility spectrometry, an ion depletion zone is set between the ionization reaction zone and the migration zone of the ion transfer tube to selectively eliminate interfering ions and improve the separation without affecting the molecules in the ionization reaction zone- ionic reaction.
背景技术Background technique
离子迁移谱（Ion Mobility Spectrometry,IMS）技术是20世纪70年代出现的一种分离检测技术，与质谱、色谱等传统技术相比，其具有结构简单、灵敏度高、分析速度快等特点，适于现场使用。离子迁移谱仪主要由电离源、离子门、迁移区和检测器组成。离子源使样品分子、N2、O2和水蒸气电离，产生的离子很容易与分子发生离子分子反应，得到多种产物离子。离子在电场的驱使下通过周期性开启的离子门进入迁移区，与逆流的中性漂气分子不断地碰撞，由于这些离子在电场中具有不同的迁移速率，使得不同的离子得到分离，先后到达检测器。Ion Mobility Spectrometry (IMS) technology is a separation and detection technology that appeared in the 1970s. Compared with traditional technologies such as mass spectrometry and chromatography, it has the characteristics of simple structure, high sensitivity, and fast analysis speed. It is suitable for Field use. Ion mobility spectrometer is mainly composed of ionization source, ion gate, migration region and detector. The ion source ionizes the sample molecules, N 2 , O 2 and water vapor, and the generated ions can easily react with the molecules to obtain various product ions. Driven by the electric field, the ions enter the migration region through the periodically opened ion gate, and continuously collide with the countercurrent neutral drift gas molecules. Because these ions have different migration rates in the electric field, different ions are separated and arrive successively. Detector.
然而，IMS的分辨率较低，迁移率接近的离子较难分离，谱图中时而出现峰重叠的现象。在载气或漂气中选择性地掺杂有机试剂是解决这一问题的手段之一。G.A.Eiceman等(G.A.Eiceman et al.,Anal.Chim.Acta,1995,306,21-33)以丙酮作为掺杂剂，显著地提高了检测19种有机磷化合物的选择性；R.Fernández-Maestre等(R.Fernández-Maestre et al.,RapidCommun.Mass Spectrom.,2012,26,2211–2223)通过对漂气进行有机溶剂的掺杂，改变了分析物的产物离子结构，从而提高了峰-峰分离度。但是，当有机试剂掺杂于载气时，其在消除干扰离子的同时也可能抑制目标化合物的电离；当有机试剂添加在漂气中时，由于离子在迁移区内与有机试剂分子间的不断碰撞，会促使离子峰的展宽。However, the resolution of IMS is low, and ions with similar mobility are difficult to separate, and peak overlaps sometimes appear in the spectra. Selective doping of organic reagents in carrier gas or drift gas is one of the means to solve this problem. G.A.Eiceman et al. (G.A.Eiceman et al., Anal.Chim.Acta, 1995,306,21-33) used acetone as a dopant, which significantly improved the selectivity of detecting 19 kinds of organophosphorus compounds; R.Fernández-Maestre etc. (R.Fernández-Maestre et al., RapidCommun.Mass Spectrom., 2012,26,2211–2223) changed the product ion structure of the analyte by doping the drift gas with an organic solvent, thus improving the peak- Peak resolution. However, when the organic reagent is doped in the carrier gas, it may suppress the ionization of the target compound while eliminating the interfering ions; Collisions will promote the broadening of ion peaks.
为了解决掺杂有机试剂所带来的问题，本发明在离子迁移管的电离反应区和迁移区之间设置离子消耗区，在离子消耗区内添加有机试剂分子，不仅可以提高分析方法的选择性和峰-峰分离度，而且不对电离反应区和迁移区造成影响。In order to solve the problems caused by the doping of organic reagents, the present invention sets an ion depletion zone between the ionization reaction zone and the migration zone of the ion transfer tube, and adds organic reagent molecules in the ion depletion zone, which can not only improve the selectivity of the analysis method and peak-to-peak resolution without affecting the ionization reaction and migration regions.
发明内容Contents of the invention
本发明公开了一种离子迁移谱分析方法，于离子迁移管的电离反应区和迁移区之间设置一个离子消耗区；离子消耗区的生成是通过在电离反应区和迁移区之间通入含有有机试剂分子的气体实现的。The invention discloses an ion mobility spectrometry analysis method. An ion depletion area is set between the ionization reaction area and the migration area of the ion transfer tube; The gas realization of organic reagent molecules.
离子迁移谱包括带接收极的离子迁移管，靠近接收极的离子迁移管一端设有漂气入口、远离接收极的离子迁移管一端设有载气入口，于漂气入口和载气入口之间的离子迁移管上设有总出气口；The ion mobility spectrometer includes an ion transfer tube with a receiving electrode. The end of the ion transfer tube near the receiving electrode is provided with a drift gas inlet, and the end of the ion transfer tube far away from the receiving electrode is provided with a carrier gas inlet. Between the drift gas inlet and the carrier gas inlet There is a total gas outlet on the ion transfer tube;
于离子迁移管的侧壁上设置有含有有机试剂分子的气体的进气口，进气口位于离子迁移管的漂气入口和总出气口之间，于进气口处的离子迁移管内形成离子消耗区，含有有机试剂分子的气体通过该进气口进入离子消耗区内。On the side wall of the ion transfer tube, there is an air inlet for gas containing organic reagent molecules. The air inlet is located between the drift gas inlet and the total gas outlet of the ion transfer tube. The depletion zone, through which gas containing organic reagent molecules enters the ion depletion zone.
迁移区和离子消耗区内气流方向一致，与电离反应区内气流方向相反；The direction of gas flow in the migration zone and the ion consumption zone is the same, and the direction of the gas flow in the ionization reaction zone is opposite;
离子迁移管内的所有气体由总出气口离开迁移管。All the gases in the ion transfer tube leave the transfer tube through the main gas outlet.
离子迁移谱为正离子模式时，有机试剂为氨、丙酮中的一种或二种以上；When the ion mobility spectrometer is in positive ion mode, the organic reagent is one or more of ammonia and acetone;
离子迁移谱为负离子模式时，有机试剂为二氯甲烷、四氯化碳中的一种或二种以上。When ion mobility spectrometry is in negative ion mode, the organic reagent is one or more of dichloromethane and carbon tetrachloride.
携带有机试剂分子的气体为空气、氮气中的一种或二种以上。The gas carrying organic reagent molecules is one or more of air and nitrogen.
含有有机试剂分子的气体中有机试剂分子的摩尔浓度为0.02-5mol/L。本发明的优点：The molar concentration of organic reagent molecules in the gas containing organic reagent molecules is 0.02-5mol/L. Advantages of the present invention:
本发明在离子迁移管的电离反应区和迁移区之间设置离子消耗区，在离子消耗区内添加有机试剂分子，不仅可以提高分析方法的选择性和峰-峰的分离度，而且不对电离反应区和迁移区造成影响。In the present invention, an ion depletion area is set between the ionization reaction area and the migration area of the ion transfer tube, and organic reagent molecules are added in the ion depletion area, which can not only improve the selectivity of the analysis method and the separation degree of peak-peak, but also prevent the ionization reaction area and migration area.
附图说明Description of drawings
图1为该方法中涉及的离子迁移管的部分结构示意图之一；Fig. 1 is one of partial structural representations of the ion transfer tube involved in the method;
图2为该方法中涉及的离子迁移管的部分结构示意图之二；Fig. 2 is the second partial structural representation of the ion transfer tube involved in the method;
图3为该方法中涉及的离子迁移管的部分结构示意图之三；Fig. 3 is the third schematic diagram of the partial structure of the ion transfer tube involved in the method;
图4为该方法中涉及的离子迁移管的部分结构示意图之四；Fig. 4 is the fourth schematic diagram of the partial structure of the ion transfer tube involved in the method;
图5为该方法中涉及的离子迁移管的部分结构示意图之五；Fig. 5 is the fifth schematic diagram of the partial structure of the ion transfer tube involved in the method;
图6a为干净空气作载气时的硫磺IMS图谱，图6b为载气中添加二氯甲烷时的硫磺IMS图谱；Figure 6a is the sulfur IMS spectrum when clean air is used as the carrier gas, and Figure 6b is the sulfur IMS spectrum when dichloromethane is added to the carrier gas;
图7为离子消耗区内加二氯甲烷的硫磺IMS图。Figure 7 is an IMS diagram of sulfur with dichloromethane added in the ion depletion region.
具体实施方式Detailed ways
本发明公开了一种的离子迁移谱分析方法，于离子迁移管的电离反应区和迁移区之间设置一个离子消耗区；离子消耗区的生成是通过在电离反应区和迁移区之间通入含有有机试剂分子的气体实现的。The invention discloses an ion mobility spectrometry analysis method. An ion depletion area is set between the ionization reaction area and the migration area of the ion transfer tube; the generation of the ion depletion area is through the Realized by a gas containing molecules of an organic reagent.
离子迁移谱包括带接收极的离子迁移管，靠近接收极的离子迁移管一端设有漂气入口、远离接收极的离子迁移管一端设有载气入口，于漂气入口和载气入口之间的离子迁移管上设有总出气口；The ion mobility spectrometer includes an ion transfer tube with a receiving electrode. The end of the ion transfer tube near the receiving electrode is provided with a drift gas inlet, and the end of the ion transfer tube far away from the receiving electrode is provided with a carrier gas inlet. Between the drift gas inlet and the carrier gas inlet There is a total gas outlet on the ion transfer tube;
于离子迁移管的侧壁上设置有含有有机试剂分子的气体的进气口，进气口位于离子迁移管的漂气入口和总出气口之间，于进气口处的离子迁移管内形成离子消耗区，含有有机试剂分子的气体通过该进气口进入离子消耗区内。On the side wall of the ion transfer tube, there is an air inlet for gas containing organic reagent molecules. The air inlet is located between the drift gas inlet and the total gas outlet of the ion transfer tube. The depletion zone, through which gas containing organic reagent molecules enters the ion depletion zone.
迁移区和离子消耗区内气流方向一致，与电离反应区内气流方向相反；The direction of gas flow in the migration zone and the ion consumption zone is the same, and the direction of the gas flow in the ionization reaction zone is opposite;
离子迁移管内的所有气体由总出气口离开迁移管。All the gases in the ion transfer tube leave the transfer tube through the main gas outlet.
离子迁移谱为正离子模式时，有机试剂为氨、丙酮中的一种或二种以上；When the ion mobility spectrometer is in positive ion mode, the organic reagent is one or more of ammonia and acetone;
离子迁移谱为负离子模式时，有机试剂为二氯甲烷、四氯化碳中的一种或二种以上。When ion mobility spectrometry is in negative ion mode, the organic reagent is one or more of dichloromethane and carbon tetrachloride.
携带有机试剂分子的气体为空气、氮气中的一种或二种以上。The gas carrying organic reagent molecules is one or more of air and nitrogen.
含有有机试剂分子的气体中有机试剂分子的摩尔浓度为0.02-5mol/L。The molar concentration of organic reagent molecules in the gas containing organic reagent molecules is 0.02-5mol/L.
如图1-5所示的该方法中涉及的离子迁移管的部分结构示意图，1为载气，2为电离反应区，3为导电环，4为绝缘环，5为总出气口，6为有机试剂气体进气口，7为离子门，8为漂气，9为离子消耗区。As shown in Figure 1-5, the partial structural diagram of the ion transfer tube involved in this method, 1 is the carrier gas, 2 is the ionization reaction area, 3 is the conductive ring, 4 is the insulating ring, 5 is the total gas outlet, and 6 is the Organic reagent gas inlet, 7 is the ion gate, 8 is the drift gas, and 9 is the ion consumption area.
图1中,含有有机试剂分子的气体进气口为1个，进气口气流方向与总出气口的气流方向呈180度；In Fig. 1, there is one gas inlet containing organic reagent molecules, and the gas flow direction of the gas inlet is 180 degrees to the gas flow direction of the total gas outlet;
图2中,含有有机试剂分子的气体进气口为1个，进气口气流方向与总出气口的气流方向呈0度；In Fig. 2, there is one gas inlet containing organic reagent molecules, and the gas flow direction of the gas inlet and the gas flow direction of the total gas outlet are 0 degrees;
图3中,含有有机试剂分子的气体进气口为2个，其中一个进气口气流方向与总出气口的气流方向呈180度，另一个进气口气流方向与总出气口的气流方向呈0度；In Fig. 3, there are two gas inlets containing organic reagent molecules, and the airflow direction of one inlet is 180 degrees to the airflow direction of the total gas outlet, and the airflow direction of the other inlet is 180 degrees to the airflow direction of the total gas outlet. 0 degree;
图4中,含有有机试剂分子的气体进气口为4个，4个进气口根据离子迁移管的中心线进行等角度的圆周分布。In Fig. 4, there are 4 gas inlets containing organic reagent molecules, and the 4 gas inlets are distributed in an equiangular circle according to the center line of the ion transfer tube.
图5中,含有有机试剂分子的气体进气口为1个，设置有该进气口的绝缘环内设有腔体，该腔体与进气口相通，并通过一系列小孔与离子消耗区相通。In Fig. 5, there is one gas inlet containing organic reagent molecules, and a cavity is provided in the insulating ring provided with the gas inlet, which communicates with the gas inlet and consumes ions through a series of small holes. The area is connected.
样品由载气携带进入电离反应区被电离，所有离子在电场的作用下经过离子消耗区，干扰离子在有机试剂分子的作用下被消除。随后，离子通过周期性开启的离子门进入迁移区，按照迁移率的差异先后到达接收极。The sample is carried by the carrier gas into the ionization reaction area and is ionized. All ions pass through the ion consumption area under the action of the electric field, and the interfering ions are eliminated under the action of organic reagent molecules. Subsequently, the ions enter the migration region through the periodically opened ion gate, and arrive at the receiving electrode successively according to the difference in mobility.
实施例1Example 1
采用IMS对S进行检测，载气在干净空气和掺杂二氯甲烷的空气间周期性切换，S的信号强度随时间的变化如图6a所示，S的IMS图谱如图6b所示。结果表明：当载气未掺杂二氯甲烷时，IMS的反应离子为氧离子（图中氯离子峰的存在是因为载气切换为干净空气后，迁移管内部仍残留有二氯甲烷），硫磺分子和氧离子反应后可以生成硫离子，但是两种离子的迁移时间很接近，出现了重叠峰；当载气中掺杂二氯甲烷时，IMS的反应离子大部分为氯离子，硫磺分子不能与氯离子反应生成硫离子，检测不到S的信号。S was detected by IMS, and the carrier gas was periodically switched between clean air and air doped with methylene chloride. The signal intensity of S changed with time as shown in Figure 6a, and the IMS spectrum of S was shown in Figure 6b. The results show that: when the carrier gas is not doped with dichloromethane, the reactive ion of IMS is oxygen ion (the existence of the chloride ion peak in the figure is because there is still dichloromethane inside the transfer tube after the carrier gas is switched to clean air), Sulfur molecules can react with oxygen ions to generate sulfur ions, but the migration time of the two ions is very close, and overlapping peaks appear; when the carrier gas is doped with dichloromethane, most of the reaction ions of IMS are chloride ions, and the sulfur molecules It cannot react with chloride ions to generate sulfide ions, and the signal of S cannot be detected.
如图7所示，当二氯甲烷添加于离子消耗区内时，IMS的反应离子为氧离子，硫分子和氧离子在电离反应区内发生反应，生成硫离子后与剩余的氧离子一起进入离子消耗区，在此区域内氧离子可以被二氯甲烷反应殆尽，最终仅剩硫离子和氯离子进入迁移区，因此IMS图上峰-峰的分离度得到了明显的提高。As shown in Figure 7, when dichloromethane is added in the ion depletion region, the reaction ion of IMS is oxygen ion, sulfur molecules and oxygen ions react in the ionization reaction region, and the sulfur ion enters together with the remaining oxygen ions Ion depletion region, in which oxygen ions can be completely reacted by dichloromethane, and finally only sulfur ions and chloride ions enter the migration region, so the peak-to-peak resolution on the IMS graph has been significantly improved.
本发明离子消耗区内含有特定的有机试剂分子，可以选择性地消除干扰离子，不仅提高了目标离子的分离度，而且避免了对电离反应区和迁移区的影响。The ion depletion area of the present invention contains specific organic reagent molecules, which can selectively eliminate interference ions, not only improves the separation degree of target ions, but also avoids the impact on the ionization reaction area and migration area.
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| CN110646501A (en) * | 2019-10-31 | 2020-01-03 | 大连大学 | A kind of method for detecting environmental hormone dimethyl phthalate |
| CN111089895A (en) * | 2019-11-29 | 2020-05-01 | 大连大学 | Application of ion mobility spectrometry in rapid detection of phthalates in plastics |
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