Fatty alcohol compound mass spectrometry method and system based on rapid derivatization reaction
By utilizing the reaction of triethylamine with sulfuryl fluoride gas in a liquid chromatography vial to generate positively charged derivatized products, the complexity and high cost of detecting fatty alcohols in existing technologies have been solved, enabling rapid, simple, and highly sensitive mass spectrometry analysis.
Patent Information
- Application Number
- CN202511441188.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-10
- Publication Date
- 2025-11-28
AI Technical Summary
Existing mass spectrometry methods for analyzing fatty alcohols suffer from problems such as cumbersome pretreatment procedures, demanding derivatization conditions, uneven derivatization efficiency, and high environmental and safety risks, leading to increased detection difficulty and costs.
Triethylamine and sulfuryl fluoride gas are reacted with fatty alcohol compounds in a liquid phase vial to generate positively charged triethylamine-substituted derivatized products via fluorosulfate intermediates. High-resolution mass spectrometry is used for qualitative analysis, which simplifies the derivatization process and is suitable for routine sample pretreatment in the laboratory.
It enables rapid derivatization and high-sensitivity detection of fatty alcohols, shortens reaction time, reduces experimental costs, and is applicable to the detection of both long-chain and short-chain fatty alcohols, thus improving the accuracy and accessibility of detection.
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Figure CN121027374A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of fatty alcohol compound detection technology, and particularly relates to a method and system for mass spectrometry analysis of fatty alcohol compounds based on rapid derivatization reaction. Background Technology
[0002] Fatty alcohols are a class of organic compounds containing long-chain alkyl and hydroxyl functional groups, playing important roles in various life processes and forming a crucial chemical basis for the complexity of life. For example, some fatty alcohols (such as phytol) are oxidized to acetyl-CoA, which enters the tricarboxylic acid cycle to produce ATP; eicosapentaenol derivatives can generate the anti-inflammatory mediator resolvins, promoting inflammation resolution; triacontanol in beeswax participates in colony communication as an insect pheromone. Recent studies have shown that there are certain differences in the content of fatty alcohols between cancerous and normal tissues, making the detection of these compounds of significant importance.
[0003] However, since fatty alcohol molecules do not absorb ultraviolet light and are not easily ionized, they are not suitable for separation by gas chromatography, making the detection and analysis of fatty alcohol compounds quite difficult. Therefore, it is necessary to develop methods that can achieve rapid analysis of these compounds.
[0004] Derivatization-based mass spectrometry is a commonly used method to enhance the detection sensitivity of poorly ionized compounds. Introducing easily ionized basic heteroatoms or charged functional groups into the target analyte structure through chemical reactions can significantly improve the mass spectrometric signal of alcohols. While existing derivatization mass spectrometry methods for aliphatic alcohols have developed into many categories, the following problems still exist: Cumbersome pretreatment procedures: Some low-polarity aliphatic alcohols require multiple derivatization steps (e.g., oxidation followed by silanization), taking several hours and increasing the risk of sample loss (e.g., volatilization, adsorption). Harsh derivatization conditions: Derivatization reactions require high temperatures (>70℃) or an anhydrous environment, which is incompatible with thermally unstable aliphatic alcohols (e.g., phytol containing double bonds), leading to degradation or isomerization. Inconsistent derivatization efficiency: Long-chain aliphatic alcohols (e.g., C20 and above) have significantly lower derivatization efficiency than short-chain aliphatic alcohols (e.g., C8-C12) due to steric hindrance and low reactivity. It poses certain environmental and safety risks: commonly used derivatization reagents (such as PFPA, MTBSTFA) are highly corrosive or carcinogenic, requiring strict protection for laboratory personnel and increasing the cost of waste liquid treatment. Summary of the Invention
[0005] To address the problems existing in the prior art, this invention provides a mass spectrometry analysis method and system for fatty alcohol compounds based on rapid derivatization reactions.
[0006] This invention is achieved by a mass spectrometry analysis method and system for fatty alcohol compounds based on rapid derivatization reaction. In the presence of triethylamine and sulfuryl fluoride gas, the hydroxyl groups of fatty alcohol compounds undergo a derivatization reaction, generating a positively charged triethylamine-substituted derivatized product via a fluorosulfate intermediate. The derivatized product is then qualitatively analyzed using a high-resolution mass spectrometer.
[0007] Furthermore, the reaction is carried out in a liquid-phase vial, first by injecting triethylamine and thioyl fluoride gas, and then by injecting a fatty alcohol solution.
[0008] Furthermore, the liquid phase vial is vortexed for 30 seconds and then allowed to stand for 10 to 60 minutes.
[0009] This invention also provides a mass spectrometry analysis system for fatty alcohols based on rapid derivatization reactions, comprising: An injection module is used to inject triethylamine and sulfuryl fluoride gas sequentially into a liquid phase vial, and to inject a fatty alcohol solution into the liquid phase vial. An oscillation module is used to perform vortex oscillation on the liquid phase vial and allow it to stand for a period of time. The qualitative analysis module is used to perform qualitative analysis of the derivatized products in the liquid chromatography vial using a high-resolution mass spectrometer.
[0010] Furthermore, the qualitative analysis module is an ultra-high performance liquid chromatography-high resolution mass spectrometry system.
[0011] Furthermore, the injection module includes a gas inlet for gas injection and an injection port for liquid injection.
[0012] Furthermore, the oscillation module is a vortex oscillation device.
[0013] This invention proposes a mass spectrometry method for the analysis of fatty alcohols based on rapid derivatization reactions. Utilizing the reactivity of the hydroxyl groups in fatty alcohol molecules, derivatization can be achieved under mild conditions through the interaction of triethylamine and thiofluoride gases. The entire process can be carried out in a liquid chromatography vial, requiring no complex pretreatment steps or expensive derivatization reagents. It is simple to operate and suitable for routine laboratory sample pretreatment procedures.
[0014] This method's derivatization process only requires vortexing for tens of seconds and settling for several minutes to complete the conversion of fatty alcohols into quaternary ammonium salt derivatization products, significantly shortening the reaction time compared to traditional esterification or silanization methods. Due to the rapid nucleophilic substitution reaction at the gas-liquid interface, the reaction kinetics are high, with few byproducts, significantly improving the overall efficiency of sample processing.
[0015] By converting neutral hydroxyl groups into positively charged quaternary ammonium functional groups, this invention effectively solves the problems of low ionization efficiency and poor signal response of fatty alcohols under electrospray ionization conditions. The derivatized fatty alcohols can generate stable and strong molecular ion peaks in high-resolution mass spectrometry, significantly improving the signal-to-noise ratio and thus greatly enhancing detection sensitivity and the accuracy of qualitative and quantitative analysis.
[0016] The method of this invention is not only applicable to the detection of long-chain fatty alcohols, but also enables rapid derivatization and effective detection of fatty alcohols with different structural types, such as short-chain fatty alcohols and secondary alcohols. It is highly versatile, covering various application scenarios such as food analysis, environmental monitoring, and biological sample analysis, and has broad industrial application potential.
[0017] The reagents used, triethylamine and thioyl fluoride, are both inexpensive and readily available chemicals. The derivatization step requires no expensive equipment or special conditions, resulting in low experimental costs and easy application in existing detection systems. Combining its advantages of simple operation, rapid reaction, high sensitivity, and wide applicability, the method of this invention can significantly improve the accessibility and practicality of mass spectrometry detection of fatty alcohols, possessing significant economic and social value.
[0018] This invention utilizes the derivatization reaction of alcohol hydroxyl groups to convert them into positively charged quaternary ammonium functional groups. The derivatization process only requires the introduction of inexpensive and readily available triethylamine and a small amount of sulfuryl fluoride gas into the substrate solution, followed by vortexing and settling. The reaction can be carried out rapidly in a liquid chromatography vial. The derivatized products exhibit good mass spectrometric response and high sensitivity. The derivatization method provided by this invention has a wide range of applications, enabling rapid derivatization of short-chain fatty alcohols, long-chain fatty alcohols, and secondary alcohols, thus facilitating rapid qualitative analysis. Attached Figure Description
[0019] Figure 1 This is a flowchart of a mass spectrometry analysis method for fatty alcohols based on rapid derivatization reaction provided in an embodiment of the present invention.
[0020] Figure 2 This is a structural block diagram of a mass spectrometry analysis system for fatty alcohols based on rapid derivatization reaction provided in an embodiment of the present invention.
[0021] Figure 3 This is a high-resolution mass spectrum obtained after octadecyl alcohol derivatization according to an embodiment of the present invention.
[0022] Figure 4 This invention provides a total ion chromatogram and expected target signal ([M+H]+) when the octadecyl alcohol solution is directly subjected to liquid chromatography-mass analysis according to an embodiment of the invention. m / z Total ion chromatogram of 271.2996 ions, with no target signal peak appearing.
[0023] Figure 5This is a high-resolution mass spectrum obtained after hexadecyl alcohol derivatization according to an embodiment of the present invention.
[0024] Figure 6 This invention provides a total ion chromatogram and expected target signal ([M+H]+) when the cetyl alcohol solution is directly subjected to liquid chromatography-mass analysis. m / z Total ion chromatogram of 243.2683 ions, with no target signal peak appearing.
[0025] Figure 7 This is a high-resolution mass spectrum obtained after oleyl alcohol derivatization according to an embodiment of the present invention.
[0026] Figure 8 This invention provides a total ion chromatogram and expected target signal ([M+H]+) for direct liquid chromatography-mass analysis of an oil-alcohol solution. m / z Total ion chromatogram of 269.2839 ions, with no target signal peak appearing.
[0027] Figure 9 This is a high-resolution mass spectrum obtained after derivatization with n-octanol, as provided in an embodiment of the present invention.
[0028] Figure 10 The present invention provides a total ion chromatogram and expected target signal ([M+H]+) when the n-octanol solution is directly subjected to liquid chromatography-mass spectrometry analysis. m / z Total ion chromatogram of 131.1431 ions, with no target signal peak appearing.
[0029] Figure 11 This is a high-resolution mass spectrum obtained after derivatization with n-heptanol, as provided in an embodiment of the present invention.
[0030] Figure 12 This invention provides a total ion chromatogram and expected target signal ([M+H]+) when directly performing liquid chromatography-mass analysis on a heptanol solution. m / z Total ion chromatogram of 117.1274 ions, with no target signal peak appearing.
[0031] Figure 13 This is a high-resolution mass spectrum obtained after 2-decyl alcohol derivatization provided in the embodiments of the present invention.
[0032] Figure 14 This invention provides a total ion chromatogram and expected target signal ([M+H]+) when directly performing liquid chromatography-mass analysis on a 2-decyl alcohol solution. m / z Total ion chromatogram of 159.1744 ions, with no target signal peak appearing. Detailed Implementation
[0033] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.
[0034] like Figure 1 As shown, the mass spectrometry analysis method and system for fatty alcohols based on rapid derivatization reaction provided in this embodiment of the invention includes the following steps: S101, triethylamine and thiosulfate gas are injected sequentially into a 2 ml liquid chromatography vial; S102, inject the fatty alcohol solution into the liquid chromatography vial using a syringe; S103, vortex oscillation for 30 seconds, then stand for 10-60 minutes; S104. High-resolution mass spectrometry was used to perform qualitative analysis on the derivatized products in the liquid chromatography vial.
[0035] Chemical reaction formula for derivatization process: The working principle, chemical transformation, and advantages of the mass spectrometry analysis method for fatty alcohols based on rapid derivatization reaction of this invention are described below: First: The basic principles of derivatization reactions The hydroxyl group (–OH) in fatty alcohol molecules exhibits low ionization efficiency and weak signal response in mass spectrometry, hindering trace detection. By introducing thiosulfate fluoride (SO₂F₂) and triethylamine (NEt₃) synergistically, the hydroxyl group can be rapidly converted into a positively charged quaternary ammonium salt derivatized product. This conversion significantly enhances the ionization ability of the molecule under soft ionization conditions such as electrospray ionization (ESI), thereby improving the sensitivity of mass spectrometry detection.
[0036] Second: Chemical transformation of derivatization reaction In the initial stage of the reaction, triethylamine acts as a base to capture the hydroxyl proton of the fatty alcohol molecule, converting the hydroxyl group into a nucleophilic alkoxide anion. Subsequently, sulfuryl fluoride gas undergoes nucleophilic substitution with the alkoxide anion to generate the intermediate fluorosulfate (ROSO2F). In this process, SO2F2 not only provides an activated sulfur center but also exhibits good gas-phase stability, enabling it to rapidly combine with the alcohol hydroxyl group in solution. The generated fluorosulfate intermediate undergoes nucleophilic substitution by triethylamine, ultimately generating a positively charged triethylamine-substituted derivatized product. This positive ion exhibits a good mass spectrometry signal response and is stabilized by the fluorosulfonic acid anion, resulting in a stable and strong characteristic ion peak for the corresponding fatty alcohol in mass spectrometry detection.
[0037] Third: Advantages in mass spectrometry detection This reaction system utilizes a gas-liquid interface activation mechanism, allowing SO2F2 to rapidly dissolve in the liquid phase and contact the alcohol hydroxyl group. Combined with the strong basicity of triethylamine, the entire derivatization process is completed within tens of seconds to minutes. Compared to traditional derivatization methods (such as chloroformate esterification or silanization), SO2F2 derivatization of alcohol hydroxyl groups exhibits extremely high specificity, and excess SO2F2 escapes as a gas, without affecting the detection results. Compared to previous derivatization methods (such as thionyl chloride / pyridine derivatization), this reaction condition is mild, the reaction is rapid, and it avoids excessive byproducts and signal interference, making it more suitable for mass spectrometry analysis.
[0038] Fourth: Advantages of mass spectrometry detection The fatty alcohol derivatized products, after this rapid derivatization process, exhibit clear molecular ion peaks in high-resolution mass spectrometry (such as Orbitrap or Q-TOF) due to their fixed positive charge, resulting in a significantly improved signal-to-noise ratio. Simultaneously, the product fragmentation pathway is clear, generating predictable characteristic ions, facilitating qualitative and quantitative analysis. Therefore, this method achieves a transformation from low responsiveness to high sensitivity and from weak to strong signals for fatty alcohol compounds, providing a reliable technical pathway for the rapid detection of fatty alcohol compounds in complex samples.
[0039] The present invention provides a mass spectrometry analysis method for long-chain fatty alcohol octadecyl alcohol based on rapid derivatization reaction: Mix 0.5 mL of triethylamine, thioyl fluoride gas, and 1 mL of octadecyl alcohol solution (using dichloromethane as solvent, approximately 1 μg / mL) in a 2 mL liquid chromatography vial. Vortex for 30 seconds and let stand for 10 minutes. Place the vial directly into the autosampler of an ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HSMS) instrument for analysis. The derivatized product of octadecyl alcohol can be obtained, and the product can be confirmed using precise mass fractions. However, direct HPLC analysis of the octadecyl alcohol solution (using dichloromethane as solvent, approximately 1 μg / mL) does not detect any signal of octadecyl alcohol. High-resolution mass spectrometry data: TOF-MS m / z 354.4089 (compared to theoretical value) m / z The deviation is 1.4 ppm (354.4094).
[0040] The present invention provides a mass spectrometry analysis method for long-chain fatty alcohol cetyl alcohol based on rapid derivatization reaction: Mix 0.5 mL of triethylamine, thioyl fluoride gas, and 1 mL of cetyl alcohol solution (using dichloromethane as solvent, approximately 1 μg / mL) in a 2 mL liquid chromatography vial. Vortex for 30 seconds and let stand for 28 minutes. Place the vial directly into the autosampler of an ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HSMS) instrument for analysis. The derivatized cetyl alcohol product can be obtained, and the product can be confirmed using precise mass fractions. However, direct HPLC analysis of the cetyl alcohol solution (using dichloromethane as solvent, approximately 1 μg / mL) does not detect any cetyl alcohol signal. High-resolution mass spectrometry data: TOF-MS m / z 326.3779 (compared to theoretical value) m / z The deviation was 0.9 ppm (326.3782).
[0041] like Figure 2 As shown in the figure, an embodiment of the present invention provides a mass spectrometry analysis system for fatty alcohols based on rapid derivatization reactions, comprising: The injection module is used to sequentially inject triethylamine and thiosulfate fluoride gas into a 2 ml liquid chromatography vial; a fatty alcohol solution is injected into the liquid chromatography vial using a syringe; The oscillation module is used for vortex oscillation for 30 seconds, followed by resting for 10-60 minutes. The qualitative analysis module is used to perform qualitative analysis of derivatized products in liquid chromatography vials using a high-resolution mass spectrometer.
[0042] Specific implementation of the present invention: Example 1: Mass Spectrometry Analysis Method for Long-Chain Fatty Alcohol Octadecyl Alcohol Based on Rapid Derivatization Reaction Mix 0.5 mL of triethylamine, thioyl fluoride gas, and 1 mL of octadecyl alcohol solution (using dichloromethane as solvent, approximately 1 μg / mL) in a 2 mL liquid chromatography vial. Vortex for 30 seconds and let stand for 10 minutes. Inject the vial directly into the autosampler of an ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HSMS) instrument for analysis. The octadecyl alcohol derivatization product is obtained, and its precise mass fraction is used for confirmation. However, direct HPLC analysis of the octadecyl alcohol solution (using dichloromethane as solvent, approximately 1 μg / mL) yields no detectable signal of octadecyl alcohol.
[0043] High-resolution mass spectrometry data: TOF-MS m / z 354.4089 (compared to theoretical value) m / z (354.4094, deviation is 1.4 ppm) Figure 3 This is a high-resolution mass spectrum obtained after octadecyl alcohol derivatization according to an embodiment of the present invention.
[0044] Figure 4 This invention provides a total ion chromatogram and expected target signal ([M+H]+) when the octadecyl alcohol solution is directly subjected to liquid chromatography-mass analysis according to an embodiment of the invention. m / z Total ion chromatogram of 271.2996 ions, with no target signal peak appearing.
[0045] Example 2: Mass Spectrometry Analysis Method for Long-Chain Fatty Alcohol Cetyl Alcohol Based on Rapid Derivatization Reaction Mix 0.5 mL of triethylamine, thioyl fluoride gas, and 1 mL of cetyl alcohol solution (using dichloromethane as solvent, approximately 1 μg / mL) in a 2 mL HPLC vial. Vortex for 30 seconds and let stand for 28 minutes. Inject the vial directly into the autosampler of an UHPLC-MS / MS system for analysis. The cetyl alcohol derivatization product is obtained, and its precise mass fraction confirms the product. However, direct HPLC analysis of the cetyl alcohol solution (using dichloromethane as solvent, approximately 1 μg / mL) yields no detectable cetyl alcohol signal.
[0046] High-resolution mass spectrometry data: TOF-MS m / z 326.3779 (compared to theoretical value) m / z (326.3782, deviation is 0.9 ppm) Figure 5 This is a high-resolution mass spectrum obtained after hexadecyl alcohol derivatization according to an embodiment of the present invention.
[0047] Figure 6 This invention provides a total ion chromatogram and expected target signal ([M+H]+) when the cetyl alcohol solution is directly subjected to liquid chromatography-mass analysis. m / z Total ion chromatogram of 243.2683 ions, with no target signal peak appearing.
[0048] Example 3: Mass Spectrometry Analysis Method for Long-Chain Fatty Alcohols Based on Rapid Derivatization Reaction Mix 0.5 mL of triethylamine, thioyl fluoride gas, and 1 mL of oleyl alcohol solution (using dichloromethane as solvent, 1 μg / mL) in a 2 mL liquid chromatography vial. Vortex for 10 seconds and let stand for 30 minutes. Inject the vial directly into the autosampler of an ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HSMS) instrument for analysis. The derivatized oleyl alcohol product is obtained, and its precise mass fraction is used for confirmation. However, direct HPLC analysis of the oleyl alcohol solution (using dichloromethane as solvent, approximately 1 μg / mL) yields no detectable signal of oleyl alcohol.
[0049] High-resolution mass spectrometry data: TOF-MS m / z 352.3944 (compared to theoretical value) m / z (352.3938 deviation is 1.7 ppm) Figure 7 This is a high-resolution mass spectrum obtained after oleyl alcohol derivatization according to an embodiment of the present invention.
[0050] Figure 8This invention provides a total ion chromatogram and expected target signal ([M+H]+) for direct liquid chromatography-mass analysis of an oil-alcohol solution. m / z Total ion chromatogram of 269.2839 ions, with no target signal peak appearing.
[0051] Example 4: Mass Spectrometry Analysis Method for n-Octanol Based on Rapid Derivatization Reaction Mix 0.5 mL of triethylamine, sulfuryl fluoride gas, and 1 mL of n-octanol solution (using dichloromethane as solvent, approximately 1 μg / mL) in a 2 mL liquid chromatography vial. Vortex for 10 seconds and let stand for 38 minutes. Inject the vial directly into the autosampler of an ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HSMS) instrument for analysis. The derivatized product of n-octanol can be obtained, and the product is confirmed using precise mass fractions. However, direct HPLC analysis of the n-octanol solution (using dichloromethane as solvent, approximately 1 μg / mL) fails to detect the target signal.
[0052] High-resolution mass spectrometry data: TOF-MS m / z 214.2527 (compared to theoretical value) m / z 214.2530 (deviation of 1.4 ppm) Figure 9 This is a high-resolution mass spectrum obtained after derivatization with n-octanol, as provided in an embodiment of the present invention.
[0053] Figure 10 The present invention provides a total ion chromatogram and expected target signal ([M+H]+) when the n-octanol solution is directly subjected to liquid chromatography-mass spectrometry analysis. m / z Total ion chromatogram of 131.1431 ions, with no target signal peak appearing.
[0054] Example 5: Mass Spectrometry Analysis Method for n-Heptanol Based on Rapid Derivatization Reaction Mix 0.5 mL of triethylamine, thioyl fluoride gas, and 1 mL of n-heptanol solution (using dichloromethane as solvent, approximately 1 μg / mL) in a 2 mL HPLC vial, vortex for 10 seconds, and let stand for 40 minutes. Inject the vial directly into the autosampler of an UHPLC-MS / MS system for analysis. The derivatized product of n-heptanol can be obtained, and the product is confirmed using precise mass fractions. However, direct HPLC analysis of the n-octanol solution (using dichloromethane as solvent, approximately 1 μg / mL) fails to detect the target signal.
[0055] High-resolution mass spectrometry data: TOF-MS m / z 200.2376 (compared to theoretical value) m / z (200.2373 deviation is 1.5ppm) Figure 11 This is a high-resolution mass spectrum obtained after derivatization with n-heptanol, as provided in an embodiment of the present invention.
[0056] Figure 12 This invention provides a total ion chromatogram and expected target signal ([M+H]+) when directly performing liquid chromatography-mass analysis on a heptanol solution. m / z Total ion chromatogram of 117.1274 ions, with no target signal peak appearing.
[0057] Example 6: Mass Spectrometry Analysis Method for 2-Decanol Based on Rapid Derivatization Reaction Mix 0.5 mL of triethylamine, thioyl fluoride gas, and 1 mL of 2-decyl alcohol solution (using dichloromethane as solvent, approximately 1 μg / mL) in a 2 mL liquid chromatography vial. Vortex for 10 seconds and let stand for 60 minutes. Inject the vial directly into the autosampler of an ultra-high performance liquid chromatography-high resolution mass spectrometry (UHPLC-MS / MS) instrument for analysis. The derivatized product of 2-decyl alcohol is obtained, and the product is confirmed using precise mass fractions. However, direct HPLC analysis of the n-octanol solution (using dichloromethane as solvent, approximately 1 μg / mL) fails to detect the target signal.
[0058] High-resolution mass spectrometry data: TOF-MS m / z 242.2846 (compared to theoretical value) m / z 242.2843 (deviation of 1.2 ppm) Figure 13 This is a high-resolution mass spectrum obtained after 2-decyl alcohol derivatization provided in the embodiments of the present invention.
[0059] Figure 14 This invention provides a total ion chromatogram and expected target signal ([M+H]+) when directly performing liquid chromatography-mass analysis on a 2-decyl alcohol solution. m / z Total ion chromatogram of 159.1744 ions, with no target signal peak appearing.
[0060] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any modifications, equivalent substitutions, and improvements made by those skilled in the art within the scope of the technology disclosed in the present invention, and within the spirit and principles of the present invention, should be covered within the scope of protection of the present invention.
Claims
1. A mass spectrometry analysis method and system for fatty alcohols based on rapid derivatization reactions, characterized in that, In the presence of triethylamine and sulfuryl fluoride gas, the hydroxyl groups of fatty alcohol compounds undergo a derivatization reaction, generating a positively charged triethylamine-substituted derivatized product via a fluorosulfate intermediate. The derivatized product is then qualitatively detected using high-resolution mass spectrometry. Specific methods: S101, triethylamine and thiosulfate gas are injected sequentially into a 2 ml liquid chromatography vial; S102, inject the fatty alcohol solution into the liquid chromatography vial using a syringe; S103, vortex oscillation for 30 seconds, then stand for 10-60 minutes; S104. High-resolution mass spectrometry was used to perform qualitative analysis on the derivatized products in the liquid chromatography vial.
2. The method according to claim 1, characterized in that, The reaction was carried out in a liquid-phase vial, first by injecting triethylamine and thioyl fluoride gas, and then by injecting a fatty alcohol solution.
3. The method according to claim 1, characterized in that, Vortex the liquid vial for 30 seconds and let it stand for 10 to 60 minutes.
4. A mass spectrometry method for analyzing long-chain fatty alcohols based on rapid derivatization reactions, characterized in that, Triethylamine and sulfuryl fluoride gas were first injected, followed by a solution containing long-chain fatty alcohols. After vortexing and static reaction, positively charged derivatized products of long-chain fatty alcohols were obtained, and the samples were analyzed and their mass numbers were confirmed by ultra-high performance liquid chromatography-high resolution mass spectrometry.
5. The method according to claim 4, characterized in that, The long-chain fatty alcohol is octadecyl alcohol, and the deviation between the mass spectrometry detection signal after derivatization and the theoretical mass number does not exceed 5 ppm.
6. The method according to claim 4, characterized in that, The long-chain fatty alcohol is hexadecyl alcohol, and the deviation between the mass spectrometry detection signal after derivatization and the theoretical mass number does not exceed 5 ppm.
7. The method according to claim 4, characterized in that, The long-chain fatty alcohol is an oleic alcohol, and the deviation between the mass spectrometry detection signal after derivatization and the theoretical mass number does not exceed 5 ppm.
8. A mass spectrometry analysis system for fatty alcohols based on rapid derivatization reactions, characterized in that, include: An injection module is used to inject triethylamine and sulfuryl fluoride gas sequentially into a liquid phase vial, and to inject a fatty alcohol solution into the liquid phase vial. An oscillation module is used to perform vortex oscillation on the liquid phase vial and allow it to stand for a period of time. The qualitative analysis module is used to perform qualitative analysis on the derivatized products in the liquid chromatography vial using a high-resolution mass spectrometer; The qualitative analysis module is an ultra-high performance liquid chromatography-high resolution mass spectrometry system.
9. The system according to claim 8, characterized in that, The injection module includes a gas inlet for gas injection and an injection port for liquid injection.
10. The system according to claim 8, characterized in that, The oscillation module is a vortex oscillation device.