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Analytical use and method of sulfhydryl nucleophilic substitution derivatization reagents

A derivatization reagent and derivatization technology, applied in the field of analytical chemistry, can solve problems such as poor stability of analytical methods, difficult accurate determination of mustard gas prototypes, and difficult real content.

Active Publication Date: 2016-09-14
INST OF PHARMACOLOGY & TOXICOLOGY ACAD OF MILITARY MEDICAL SCI P L A
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, mustard gas is a highly active alkylating agent. In complex environmental samples or biological samples, most of its prototype molecules are easily degraded, hydrolyzed or rapidly undergo biotransformation such as addition, which makes it difficult to accurately determine the prototype mustard gas. True content in complex samples has been a major challenge associated with this field of analysis
[0004] At present, gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) are the main methods for the detection of mustard gas and its related compounds, but there are shortcomings such as poor stability of the analytical method, complicated sample pretreatment, and unsuitability for biological sample analysis.
Although liquid chromatography (LC) and liquid chromatography-mass spectrometry (LC-MS) have the advantages of simple sample pretreatment and high sensitivity, due to the combination of mustard gas and its oxidation product mustard sulfone, etc. Alkylation or hydrolysis reactions occur in the column packing and flow phase, so it is generally believed that liquid chromatography cannot be directly used to analyze mustard gas prototypes and related compounds

Method used

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  • Analytical use and method of sulfhydryl nucleophilic substitution derivatization reagents
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  • Analytical use and method of sulfhydryl nucleophilic substitution derivatization reagents

Examples

Experimental program
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Effect test

preparation example 1

[0070] Preparation Example 1: Preparation and Characterization of S,S'-Diacetyltrithiodiglycol

[0071] 5% mustard gas acetonitrile solution was added to 0.1g / mL PTA aqueous solution in portions or once, sealed with a polytetrafluoroethylene (PTFE) bottle cap, and reacted at 100°C for 1 hour; the reaction mixture was extracted with 2mL dichloromethane , the extract was subjected to silica gel column chromatography, the eluting solvent was n-hexane:dichloromethane=1:3, the collected fractions were subjected to vacuum distillation to obtain the derivative product S,S'-diacetyl trisulfide of mustard gas and PTA Diethylene glycol.

[0072] figure 1 S,S'-Diacetyltrithiodiglycol 1 H NMR spectrum. The characterization results showed that the purity of the refined S,S'-diacetyltrithiodiglycol could meet the experimental requirements.

preparation example 2

[0073] Preparation Example 2: Preparation and Characterization of 3,5-Dimercaptomethyl-Phenoxyacetic Acid

[0074] The preparation method of 3,5-dimercaptomethyl-aromatic compound is as follows:

[0075]

[0076] The dithiol derivatization reagent 3,5-dimercaptomethyl-phenoxyacetic acid (DSH) was prepared and purified according to the above synthetic route.

[0077] figure 2 for DSH 1 H NMR spectrum. The characterization results showed that the purity of the prepared DSH could meet the experimental requirements.

Embodiment 1

[0078] Embodiment 1: the instrument parameter optimization of PTA derivatization method

[0079] Prepare PTA aqueous solution and d4-mustard acetonitrile internal standard solution with a concentration of 0.1 mg / mL and 1 mg / mL respectively, mix the sample containing mustard gas with PTA solution and internal standard solution, vortex and mix, and place in a water bath at 50°C Reacted for 30min, the reaction solution was centrifuged at 14000rpm for 10 minutes, 50 μL of supernatant was put into the intubation tube of the sampling bottle, and the chromatograms of mustard gas and d4-mustard gas were measured with a triple quadrupole linear ion trap tandem mass spectrometer (LC / MS Hyphenated instrument 5500QTRAP, equipped with TurboV electrospray ionization source (ESI) and ACQUITY TM ultra-high performance liquid chromatography (UPLC).

[0080] The detection conditions of liquid chromatography-mass spectrometry are as follows:

[0081] Chromatographic conditions Chromatographi...

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Abstract

The present invention is the use of cymbal -based derivatives in the field of chemical chemistry, which is used in the detection of mustard gas and its related compound detection.The invention also involves a method of detecting mustard gas and / or its related compounds.Specifically, the detection method includes the following steps: use the cymbal derivative reagent, or to add a pyrometer derivative reagent to the samples to the samples that pass or have not been prepared.The present invention is suitable for the measurement of highly reflected lively and lively mustard gas and related compound prototypes, which overcome the disadvantages of inaccurate prototypes or content measurement of mustard gas, nitrogen mustard in complex samples due to rapid hydrolysis or alkylated conversion.It is good and stable. It can be used in environmental samples and biological samples that have reactionary mustard gas and related compound liquid chromatography.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to the application of mercapto derivatization reagents in the detection of mustard gas and its related compounds. The invention also relates to a method of detecting mustard gas and / or its related compounds. Background technique [0002] Mustard gas (sulfur mustard, SM), whose chemical name is 2,2'-dichlorodiethyl sulfide, is a difficult-to-prevent and intractable chemical warfare agent. It has been used many times in wars, causing a large number of casualties . At present, SM is still the main filler for the world's existing chemical weapons, and it is also the main component of Japan's abandoned chemical weapons in China. Therefore, the rapid and accurate detection of mustard gas and its related compounds has important research significance in terms of responding to public emergencies, clinical diagnosis, treatment, prognosis assessment and poisoning mechanism research of mustar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 谢剑炜徐斌吴剑峰郭磊宗成齐美玲
Owner INST OF PHARMACOLOGY & TOXICOLOGY ACAD OF MILITARY MEDICAL SCI P L A
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