Analysis method for amide compounds

A technology for amide compounds and analytical methods, applied in analytical materials, material separation, measurement devices, etc., can solve the problems of difficulty in achieving separation effects and lack of uniform standards, and achieve simple and fast analytical methods, good linearity, and good separation. effect of effect

Active Publication Date: 2014-01-15
GUANGZHOU GRG METROLOGY & TEST CO LTD
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Currently, acrylamide, N-methylacetamide, N,N-dimethylformamide, formamide, N,N-dimethylacetamide, these five amide substances are listed as highly concerned in the REACH regulations There is no unified standard for the detection of these substances. The detection of such substances is mainly by reversed-phase high-performance liquid chromatography. However, these compounds are highly polar and have similar properties, and liquid phase methods are used. Difficult to achieve good separation

Method used

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  • Analysis method for amide compounds
  • Analysis method for amide compounds
  • Analysis method for amide compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A method utilizing gas chromatography-mass spectrometry to measure amides, comprising the following steps:

[0030] A. Preparation of standard solution

[0031] Weigh a certain quality of standard solution, prepare a single standard solution of 1000mg / L, and then dilute it step by step to 0.01mg / L, 0.1mg / L, 0.5mg / L, 1mg / L, 2mg / L, 5mg / L, 10mg / L mixed standard solution.

[0032] B. Pretreatment of samples

[0033] Take the sample from the clean part of the sample, cut it into pieces below 3mm×3mm, weigh 1g±0.1g (accurate to 0.1mg) of the sample into a 60ml glass reaction bottle, add 10ml methanol, extract for 1h±5min, repeat the above operation once, and combine The two extracts were mixed evenly, concentrated with a rotary evaporator, and finally the volume was adjusted to 1ml with methanol, and the sample was filtered through a 0.45um microporous membrane to obtain the sample to be tested.

[0034] C. Selection of Gas Chromatography-Mass Spectrometry Conditions

[0...

Embodiment 2 Embodiment 1

[0052] The peak situation and qualitative and quantitative ion selection of five kinds of amide compounds in embodiment 1

[0053] Table 2 The peak time and qualitative and quantitative ions of five kinds of amide compounds

[0054]

[0055]

[0056] Through Table 2 and figure 1 It can be seen that under the analysis conditions of Example 1, the five amide compounds can be well separated.

Embodiment 3

[0057] Embodiment 3 standard working curve

[0058] Table 3 Linear equations and correlation coefficients of five kinds of amide compounds

[0059]

[0060] from Table 3 and figure 2 It can be seen that within the linear range of 0.01mg / L-10mg / L, the linear correlation coefficients of the five amides are all above 0.9995.

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Abstract

The invention discloses an analysis method for amide compounds. The analysis method adopts a gas chromatography-mass spectrometry method. According to the invention, under the optimized analysis conditions, very good chromatographic peaks of the five amide compounds can be obtained within 15 min; very good separating effects can be obtained; the linearities of all the target compounds are good within a concentration range of 0.01-10 mg/L; the correlation coefficients are all greater than 0.9995; the detection limits reach 0.01 mg/kg; the relative standard deviations are smaller than 2.5%; the recovery rates of standard addition are 80-105%. The analysis method is convenient, fast, accurate, and reliable, and can meet REACH regulation requirements on hazardous amides.

Description

technical field [0001] The invention relates to the field of chemical analysis, in particular to an analysis method for amide compounds. Background technique [0002] Acrylamide, N-methylacetamide, N,N-dimethylformamide, formamide, N,N-dimethylacetamide (see Table 1 for basic information) are all good solvents and are widely used in fiber In , leather, pharmaceutical, petroleum processing and organic synthesis industries, they can play a very good role in these fields, but after long-term research, it has been found that these amide compounds have serious toxic effects on the human body. Among them, formamide and N,N-dimethylformamide are slightly irritating to the skin and sometimes can cause allergies, and their vapor or mist can irritate the eyes, mucous membranes and upper respiratory tract. Acrylamide will combine with guanine on DNA to form adducts in vivo, leading to genetic material damage and gene mutation. N, N-dimethylacetamide poisoning is manifested as decreas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 王华任祥祥王海鸣
Owner GUANGZHOU GRG METROLOGY & TEST CO LTD
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