WO2021212920A1 - 环境固体样品溶解有机物的纳升喷雾-fticr-ms分析方法及装置 - Google Patents
环境固体样品溶解有机物的纳升喷雾-fticr-ms分析方法及装置 Download PDFInfo
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Classifications
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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
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
Definitions
- the invention relates to the technical field of natural dissolved organic matter (DOM) analysis, in particular to an analysis method and device shared by nanoliter spray and Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS).
- DOM natural dissolved organic matter
- Soil and sediment are the largest carbon pools in the terrestrial system of the earth. Most of the carbon is encapsulated in minerals or exists in the form of solid phase after long-term mineralization and stabilization.
- the solid phase contains a small amount of interstitial water, and the dissolved organic matter has Highly active, it plays a key role in the formation of soil and sediment aggregates, carbon storage, and global carbon cycle. It is also a source of microbial energy and plant nutrients nitrogen and phosphorus.
- due to the high mobility and diversity of dissolved organic matter studies have confirmed that it also has a key role in the transmission of metal ions and organic pollutants. Due to its rapid response to the environment and the source of organic matter, soil, sedimentation Dissolved organic matter can also indicate changes in land use and vegetation types.
- test of soil dissolved organic matter can be tested by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry, which is one of the highest-resolution mass spectrometers at present.
- the samples need to be purified and enriched by solid phase extraction, but the test method has the following techniques problem:
- the current general pre-processing method is to extract organic matter through the PPL column (Thorsten Dittmar, Boris Koch, Norbert Hertkorn, and Gerhard Kattner, A Simple and Efficient Method for the Solid-Phase Extraction of Dissolved Organic Matter (SPE-DOM) Seawater, Limnology and Oceanography, 6(2008), 230–35), as there may be as many as 100,000 types of dissolved organic matter, including peptides, sugars, and amorphous polymer humic acids whose structure cannot be confirmed.
- the pre-extraction processing method leads to the selective loss of characteristic organic signal (Raeke Julia, Lechtenfeld Oliver J, Wagner Martin, et al.
- the extraction loss may be as high as 90%, which also weakens the quantitative significance of the method, and the difference between different samples is reduced due to the same extraction selectivity.
- the current internationally universal mass spectrometry detection method is ionized through a general electrospray source and then enters Fourier transform ion cyclotron resonance mass spectrometry detection, but due to the obvious selective suppression problem of the electrospray source, this Method
- the ionization process may be inhibited by substances with high surface activity.
- the ionization efficiency of substances with amino acids or carbohydrates and strong polarity is significantly lower than that with surface activity. Active substance.
- the water sample required for the analysis of natural dissolved organic matter by solid phase extraction is generally larger than 20 mL, which is very difficult to sample for the soil. Therefore, the traditional method is to obtain dissolved organic matter by eluting with ultrapure water or water added with inorganic salts. , But this method does not represent the dissolved organic matter in the actual soil, but only the potentially eluted matter, and the actual eluted dissolved organic matter is related to the elution method, the amount of water added and the inorganic salt, resulting in the same sample result There is uncertainty.
- the purpose of the present invention is to provide a method and device for analyzing and detecting trace amounts of interstitial water in environmental solid samples without solid phase extraction.
- the present invention provides a nano-spray-FTICR-MS analysis device for dissolved organic matter in environmental solid samples, including a nano-spray device and Fourier transform ion cyclotron resonance mass spectrometry;
- Nano spray device includes glass nozzle, conductive needle, transfer rubber head, double pressurized ball and gas storage bag; transfer rubber head is a hollow tube structure, one end is sleeved on the end of the glass nozzle away from the nozzle, and the other end passes through
- the pipe is connected to one end of the gas storage bag, the other end of the gas storage bag is connected to one end of the double pressurized ball through the one-way valve one, and the other end of the double pressurized ball is connected to the outside air through the one-way valve two, press the double pressurized ball
- the one-way valve is opened, the one-way valve two is closed.
- the double pressurized ball is released, the one-way valve is closed and the one-way valve two is opened;
- the conductive needle is arranged on the axis of the glass nozzle, one end is close to the nozzle of the glass nozzle, the other end extends into the transfer rubber head and is connected to one end of the metal conductive clip passing through the side wall of the transfer rubber head, and the other end of the metal conductive clip is grounded;
- the sample solution loaded on the glass nozzle is a mixed solution composed of interstitial water and organic solvent, and the nozzle is aimed at the injection port of the Fourier transform ion cyclotron resonance mass spectrometer.
- the conductive needles are gold-plated steel needles or silver needles.
- the sample solution is directly injected from the adapter rubber head into the glass spray head through a micro syringe.
- the ratio of the interstitial water to the organic solvent ranges from 1:1 to 1:100,
- the organic solvent includes alcohols, and the ratio of alcohol to other organic solvents is 1:0 to 1:10.
- a pressure gauge is provided on the gas storage bag.
- the present invention provides a nano-spray-FTICR-MS analysis method of dissolved organic matter in environmental solid samples, which adopts the above-mentioned analysis device and includes the following steps:
- the sample solution is a mixed solution composed of interstitial water, methanol, and isopropanol;
- the molecular ion peaks of the dissolved organic matter include multiple types of organic matter, including lipid regions, protein or polypeptide regions, amino sugar regions, black carbon regions, lignin regions, and tannin/polyphenol regions.
- the formulation of the sample to be tested is a mixed solution of interstitial aqueous solution, methanol, and isopropanol, which can greatly improve the ionization efficiency of dissolved organics and reduce selective inhibition.
- the nano-liter spray device uses gold-plated steel needles, which are highly chemically inert and conductive.
- the device is equipped with a pressurized ball, which can achieve stable spray in the lower voltage state of the ion source.
- Figure 1 is a schematic diagram of the structure of the nanoliter spray device disclosed in the present invention.
- Fig. 2 is a schematic diagram of the combination of the nano-liter spray device disclosed in the present invention and Fourier transform ion cyclotron resonance mass spectrometry.
- FIG. 3 is a comparison diagram of different methods of the International Humic Acid Association standards (naturally dissolved organic carbon), in which:
- (b) is the Van Krevelen distribution map of organic matter obtained by using the nanoliter spray ionization source of the present invention
- (d) is the molecular weight distribution diagram of organic matter obtained by using the nanoliter spray ionization source of the present invention.
- (e) is a graph of the difference in the number of detected molecules, the white is the traditional method, the gray is the nano-spray ionization source method of the present invention, and the overlap is the shared part.
- Fig. 4 is a Van Krevelen distribution diagram of organic substances obtained by using the nanoliter spray ionization source of the present invention after 10-fold dilution of the International Humic Acid Association standard substance (natural dissolved organic carbon).
- FIG. 5 is a comparison diagram of different methods of dissolved organic matter (DOM) in interstitial water of forest soil, in which:
- (b) is the Van Krevelen distribution map of organic matter obtained by using the nanoliter spray ionization source of the present invention.
- Fig. 6 is a diagram showing the difference of the types of dissolved organic matter in water measured by the two methods.
- the dotted box shows the signal distribution of dissolved organic matter measured by the method and device of the present invention, and the dotted circle shows the signal distribution of dissolved organic matter measured by the traditional method.
- 14-lipid region 15-protein or polypeptide region; 16-amino sugar region; 17-black carbon region; 18-lignin region; 19-tannin/polyphenol region.
- this embodiment provides a nano-spray-FTICR-MS analysis device for dissolving organic matter in environmental solid samples, including a nano-spray device and Fourier transform ion cyclotron resonance mass spectrometry.
- the nanoliter spray device is installed on the fixed frame 3 as a whole, mainly including glass nozzle 1, conductive needle 2, transfer rubber head 4, double pressurized ball 5, gas storage bag 6, one-way valve 7, one-way valve two 8.
- the adapter rubber head 4 is a hollow tube structure, one end is sleeved on the end of the glass nozzle 1 away from the nozzle, the other end is connected to one end of the gas storage bag 6 through a pipe, and the other end of the gas storage bag 6 is connected to the double connection through a one-way valve 7
- One end of the pressurized ball 5 is connected, the other end of the double pressurized ball 5 is connected to the outside air through a one-way valve 8, and a pressure gauge 11 is connected to the gas storage bag 6.
- the setting of the one-way valve 7 and the one-way valve 8 is: when the double pressurized ball 5 is pressed, the one-way valve 7 opens, the one-way valve 2 8 closes, and the air in the double pressurized ball 5 is squeezed.
- the pressure enters the gas storage bag 6; when the double pressurizing ball 5 is released, the one-way valve 7 is closed, and the one-way valve two 8 is opened, and outside air is added to the double pressurizing ball 5 for the next pressurization.
- the conductive needle 2 is arranged on the axis of the glass nozzle 1, one end is close to the nozzle of the glass nozzle 1, and the other end extends into the transfer rubber head 4 to connect with one end of the metal conductive clip 10 passing through the side wall of the transfer rubber head 4, and the other end of the metal conductive clip 10 One end is grounded.
- the conductive needle 2 adopts a gold-plated steel needle or a silver needle with a high degree of chemical inertness and conductivity, which can achieve stable spraying in a lower voltage state of the ion source.
- the sample solution 13 loaded on the glass nozzle 1 is a mixed solution composed of interstitial water and an organic solvent, and the nozzle is aimed at the injection port 12 of the Fourier transform ion cyclotron resonance mass spectrometer.
- the ratio of interstitial water to organic solvent ranges from 1:1 to 1:100
- the organic solvent includes at least methanol, or other organic solvents such as isopropanol, and the ratio of methanol to other organic solvents is 1:1. 0 to 1:10.
- This embodiment provides a nano-spray-FTICR-MS analysis method of dissolved organic matter in environmental solid samples, using the analysis device described in embodiment 1, specifically including:
- the analysis method of the present invention effectively increases the type and quantity of measurable dissolved organic matter.
- Figure 4 shows the same process and method as in Example 2.
- the molecular type distribution diagram measured after the sample solution is ten times diluted.
- Figure 5 shows the distribution of dissolved organic matter when this method is applied to forest soil.
- the same process and method as in Example 2 are used.
- the sample solution is the distribution of molecular types measured after ten-fold dilution of interstitial water. You can see The same effect as the implementation example 1 appears, that is, the method detects more types of organic matter in the interstitial water of forest soil, covering lipid region 14, protein or polypeptide region 15, amino sugar region 16, black carbon region 17.
- Lignin area 18, tannin/polyphenol area 19 Figure 6
- observing the measured organic matter composition found that this method measured more nitrogen-containing organic matter, and possibly higher bioavailability sex. This shows that soil dissolved organic carbon plays a greater role in the soil carbon cycle and nitrogen cycle than previously recognized.
- the amount of sample required by this method is much lower than traditional methods, and the detectable protein-like and polysaccharide-like substances are the key targets for plant root microregion related research. Therefore, it is especially suitable for soil and sediment samples that require a high-resolution organic composition profile. In addition to soil, it can also be extended to other environmental sample types with similar concentration ranges and matrix characteristics.
- the nano-spray-FTICR-MS analysis method and device of the present invention use a nano-spray device in combination with Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS), and does not purify and enrich the sample by solid phase extraction.
- FTICR-MS Fourier transform ion cyclotron resonance mass spectrometry
- the len distribution map shows that in addition to the lignin-like area that is mainly tested by the traditional method, the lipid area, protein or peptide area, amino sugar area, black carbon area, and tannin/polyphenol area can be obtained.
- Molecule which solves the key problems of loss of biologically active molecular signals and selective signal suppression of ordinary electrospray sources through solid-phase extraction pretreatment.
- the sample volume is one ten thousandth of that of traditional methods, which can meet the requirements of environmental solid samples (such as soil, sediments, etc.) the in-situ dissolved organic matter analysis that is difficult to obtain interstitial water samples solves the problem of using elution/water extractable dissolved organic matter that cannot reflect the real environment in the past.
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Abstract
Description
Claims (8)
- 一种环境固体样品溶解有机物的纳升喷雾-FTICR-MS分析装置,其特征在于:包括纳升喷雾装置和傅立叶变换离子回旋共振质谱;纳升喷雾装置包括玻璃喷头(1)、导电针(2)、转接橡胶头(4)、双联加压球(5)和气体储存袋(6);转接橡胶头(4)为中空管腔结构,一端套接在玻璃喷头(1)远离喷嘴的一端,另一端通过管道与气体储存袋(6)一端相连,气体储存袋(6)另一端通过单向阀一(7)与双联加压球(5)一端相连,双联加压球(5)另一端通过单向阀二(8)与外界空气相连,按压双联加压球(5)时,单向阀一(7)打开,单向阀二(8)关闭,松开双联加压球(5)时,单向阀一(7)关闭,单向阀二(8)打开;导电针(2)设置在玻璃喷头(1)轴心,一端靠近玻璃喷头(1)喷嘴,另一端伸入转接橡胶头(4)与穿过转接橡胶头(4)侧壁的金属导电夹(10)一端相连,金属导电夹(10)另一端接地;玻璃喷头(1)装载的样品溶液(13)为间隙水和有机溶剂组成的混合溶液,喷嘴对准傅立叶变换离子回旋共振质谱的进样口(12)。
- 根据权利要求1所述的一种环境固体样品溶解有机物的纳升喷雾-FTICR-MS分析装置,其特征在于:所述的导电针(2)为镀金钢针或银针。
- 根据权利要求1所述的一种环境固体样品溶解有机物的纳升喷雾-FTICR-MS分析装置,其特征在于:所述的样品溶液(13)通过微量注射器直接从转接橡胶头(4)注射进入玻璃喷头(1)。
- 根据权利要求1所述的一种环境固体样品溶解有机物的纳升喷雾-FTICR-MS分析装置,其特征在于:所述的间隙水与有机溶剂的配比范围为1:1至1:100,
- 根据权利要求1所述的一种环境固体样品溶解有机物的纳升喷雾-FTICR-MS分析装置,其特征在于:所述的有机溶剂包括醇类,醇与其他有机溶剂的配比为1:0至1:10。
- 根据权利要求1所述的一种环境固体样品溶解有机物的纳升喷雾-FTICR-MS分析装置,其特征在于:所述的气体储存袋(6)上设置有压力计(11)。
- 一种环境固体样品溶解有机物的纳升喷雾-FTICR-MS分析方法,采用权利要求1-6之一所述的分析装置,其特征在于:包括以下步骤:(1)将配置好的样品溶液装入玻璃喷头中,样品溶液为间隙水、甲醇、异丙醇组成的混合溶液;(2)调节玻璃喷头对准傅立叶变换离子回旋共振质谱进样口,傅立叶变换离子回旋共振 质谱离子源加压开启,通过双联加压球吸入空气玻璃喷头开始加压,库伦爆炸实现喷雾;(3)傅立叶变换离子回旋共振质谱开始扫描并累积谱图,获得溶解有机物的准分子离子峰并进行解谱后得到分子式。
- 根据权利要求7所述的一种环境固体样品溶解有机物的纳升喷雾-FTICR-MS分析方法,其特征在于:所述溶解有机物的分子离子峰包含多种有机物类型,包括脂质区、蛋白质或多肽区、氨基糖区、黑碳类区、木质素类区、单宁类/多酚区。
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