Method for pre-column derivatization for sulfonyl isocyanic ester of hydroxyl compound and sulfhydryl commpound

A technology of sulfonyl isocyanate and pre-column derivatization, which is applied in the field of analytical chemistry, can solve the problems of no pre-column derivatization, etc., and achieve the effect of high reaction time and less side reaction products

Inactive Publication Date: 2005-08-31
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Sulfonyl isocyanate compounds, the general structure of which can be expressed as RSO 2 NCO, where R can be various groups such as alkyl, aryl, etc., was mainly used in organic synthesis in the past, and there is no report on its use in pre-column derivatization

Method used

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  • Method for pre-column derivatization for sulfonyl isocyanic ester of hydroxyl compound and sulfhydryl commpound
  • Method for pre-column derivatization for sulfonyl isocyanic ester of hydroxyl compound and sulfhydryl commpound
  • Method for pre-column derivatization for sulfonyl isocyanic ester of hydroxyl compound and sulfhydryl commpound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Instruments and Conditions

[0020] American Agilent 1100 high performance liquid chromatography system, including low pressure quaternary gradient system, online degassing, column temperature control box, variable wavelength detector, ChemStation for LC 3D workstation and 20μl manual sampling system; chromatographic column: 1 50× 4.6mm ID, 5μm Diamonsil TM C 18 (DIKMA); mobile phase A: weigh 1.79 grams of NaH 2 PO 4 2H 2 Dissolve O in 250ml of pure water, add 250ml of acetonitrile, and adjust the pH value to 2.5 with phosphoric acid; mobile phase B: weigh 1.79g of NaH 2 PO 4 2H 2 Dissolve O in 100ml of pure water, add 400ml of acetonitrile, and adjust the pH value to 2.5 with phosphoric acid; gradient program:

[0021] T(min) A(%) B(%)

[0022] 0 100 0

[0023] 20 0 100

[0024] 25 0 100

[0025] Flow rate: 1.0ml / min; Column temperature: 25°C; Detection wavelength: 227nm

[0026] Experimental procedure

[0027] Ta...

Embodiment 2

[0029] Instruments and Conditions

[0030] American Agilent 1100 HPLC-MSD high-performance liquid chromatography-mass spectrometry system, the system includes online degassing, binary high-pressure gradient system, column temperature control box, automatic sampler, diode array detector, electrospray interface (ion source), Quadrupole mass analysis system and ChemStation for LC-MS 3D workstation.

[0031] Chromatographic conditions Column: 200×4.6mm ID, 5μm Diamonsil TM C 18 (DIKMA); mobile phase A: 0.2% ammonium acetate solution (g / ml); mobile phase B: methanol; gradient elution program

[0032] T(min) A(%) B(%)

[0033] 0 22 78

[0034] 10 0 100

[0035] Flow rate: 0.8ml / min; Column temperature: 25°C

[0036] Mass spectrometry conditions ESI negative ion ionization; fragmentation voltage: 130V; spray pressure: 40psi; nitrogen flow rate: 10L / min; drying air temperature: 350°C; capillary voltage: 4000V; 1 =511.0 (Org 4094 and Org 30126), M 2...

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Abstract

In solvent not containing active hydrogen, with compound of sulfonyl isocyanic ester being as derivatization reagent, method of pre-column derivatization is carried out for hydroxyl compound and sulfhydryl compound. Then, water is added to stop reaction. The method has advantages of mild reaction condition, fast reaction speed, few side reactions and determination not affected by superfluous reagent. High-sensitivity measuring hydroxyl compound and sulfhydryl compound can be realized by combination of derivatization method with methods of high efficiency liquid chromatography, high efficiency liquid chromatograph-mass spectrum, capillary electrophoresis or capillary electrophoresis- mass spectrum.

Description

technical field [0001] The invention belongs to the field of analytical chemistry and relates to a pre-column derivatization method for compounds, in particular to a pre-column derivatization method for sulfonyl isocyanate of hydroxyl compounds and mercapto compounds. Background technique [0002] Pre-column derivatization is a common method to improve the detection sensitivity of hydroxyl compounds and mercapto compounds, but the derivatization methods of hydroxyl compounds and mercapto compounds reported so far all suffer from long reaction time, high reaction temperature, many side reaction products, and excessive Derivatization reagents interfere with the determination of side substances and other defects. Sulfonyl isocyanate compounds, the general structure of which can be expressed as RSO 2 NCO, where R can be various groups such as alkyl group and aryl group, has been mainly used in organic synthesis in the past, and there is no report on its use in pre-column deriva...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/36G01N30/40G01N30/72G01N30/88
Inventor 段更利左明
Owner FUDAN UNIV
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