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Method for measuring aromatic amine in crayons

A method for measuring aromatic amines, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of unsuitable detection of aromatic amines in crayons, and achieve the effect of avoiding matrix interference and easy method

Inactive Publication Date: 2011-10-12
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current detection methods for carcinogenic aromatic amines reported in the literature are mainly for samples made of textiles, leather and other materials, and because the composition of crayons is quite different from the above materials, the existing detection methods are not suitable for the detection of aromatic amines in crayons

Method used

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  • Method for measuring aromatic amine in crayons
  • Method for measuring aromatic amine in crayons

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Determination of aromatic amines in crayons

[0023] (1) Crayon sample processing

[0024] (1) Weigh a crayon of a certain quality, cut it into small pieces with a clean blade, use n-hexane to perform ultrasonic pretreatment on the crayon piece, discard the n-hexane, and then volatilize it to nearly dry under ventilated conditions to obtain the pretreated sample ;

[0025] (2) Use methanol to ultrasonically extract the pretreatment sample twice, and add methanol according to the ratio of 1 gram of crayon / 40ml of methanol;

[0026] (3) After centrifuging the extract, collect the clarified solution into a chicken heart bottle, and use a rotary evaporator to dry it until it is nearly dry, and then dry it with a slow nitrogen flow;

[0027] (4) Add 200mg / ml sodium dithionite solution (200mg / ml sodium dithionite solution prepared with a citrate buffer solution of pH 6 as a solvent) into the chicken heart bottle, and add dithionite at a ratio of 1 gram of crayon / 0.6 gram...

Embodiment 2

[0058] The mensuration of aromatic amine in embodiment 2, crayon

[0059] 1. Determination of aromatic amines in crayons

[0060] (1) Crayon sample processing

[0061] (1) Weigh a crayon of a certain quality, cut it into small pieces with a clean blade, use cyclohexane to perform ultrasonic pretreatment on the crayon small pieces, discard the cyclohexane, and then volatilize it to nearly dry under ventilated conditions to obtain the former processing samples;

[0062] (2) Use acetonitrile to ultrasonically extract the pretreatment sample twice, and add acetonitrile according to the ratio of 1 gram of crayon / 60ml of acetonitrile;

[0063] (3) After centrifuging the extract, collect the clarified solution into a chicken heart bottle, and use a rotary evaporator to dry it until it is nearly dry, and then dry it with a slow nitrogen flow;

[0064] (4) Add 200mg / ml sodium dithionite solution (200mg / ml sodium dithionite solution prepared with a citrate buffer solution of pH 6 as ...

Embodiment 3

[0078] The mensuration of aromatic amine in embodiment 3, crayon

[0079] 1. Determination of aromatic amines in crayons

[0080] (1) Crayon sample processing

[0081] (1) Weigh a crayon of a certain quality, cut it into small pieces with a clean blade, use heptane to perform ultrasonic pretreatment on the crayon piece, discard the heptane, and then volatilize it to nearly dry under ventilated conditions to obtain a pretreatment sample ;

[0082] (2) Use isopropanol to ultrasonically extract the pretreatment sample twice, and add isopropanol according to the ratio of 1 gram of crayon / 20ml of isopropanol;

[0083] (3) After centrifuging the extract, collect the clarified solution into a chicken heart bottle, and use a rotary evaporator to dry it until it is nearly dry, and then dry it with a slow nitrogen flow;

[0084] (4) Add 200mg / ml sodium dithionite solution (200mg / ml sodium dithionite solution prepared with a citrate buffer solution of pH 6 as a solvent) into the chick...

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Abstract

The invention discloses a method for measuring aromatic amine in crayons, which comprises the following steps of: cutting crayons into small pieces, performing ultrasonic pretreatment on samples by using normal hexane, cyclohexane or heptane, and removing the normal hexane, the cyclohexane or the heptane to obtain pretreatment samples; performing ultrasonic extraction on the pretreatment samples by using methanol, ethanol, isopropanol or acetonitrile to obtain extracting solution; removing organic solvent in the extracting solution, and adding sodium hyposulfite solution to perform a reduction reaction at the temperature of between 60 and 80 DEG C; after the reaction is finished, regulating the pH value of reaction solution to be between 7 and 9, adsorbing by a siliceous earth column, andeluting by using methyl tertiary butyl ether or diethyl ether to obtain eluent; and adding 0.5 to 1 mol / L hydrochloric acid solution into the eluent, removing an organic layer on an upper layer, regulating the pH value of a residual aqueous phase to be between 7 and 9, adding the methyl tertiary butyl ether or the diethyl ether, and after an organic phase and the aqueous phase are layered completely, extracting the organic phase to measure the aromatic amine in a gas chromatograph-mass spectrometer. The method disclosed by the invention fills the blank of the technology, and the problem of matrix interference caused by other ingredients in the crayons is solved effectively.

Description

technical field [0001] The invention relates to a method for determining aromatic amines in crayons. Background technique [0002] The main ingredients in crayons are waxes, vaseline, mineral oil, calcium carbonate, stearic acid, dyes, etc. Due to the unqualified production process and unqualified raw materials, some harmful substances will remain in the crayons, the most important of which are carcinogenic aromatic amines. Such substances mainly come from the decomposition of certain azo dyes in crayons. If these azo dyes are used in the crayon manufacturing process, then when the crayons come into direct contact with the human body, these substances will be released in human metabolites (such as sweat, saliva, etc.) ) to decompose aromatic amines, which are absorbed by the human body and cause health hazards. In the EN71 series of standards formulated by the European Standardization Committee, it is stipulated that no more than 5mg / kg of aniline o-toluidine, 2-methoxyani...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/14
Inventor 张庆白桦康苏媛吕庆王超
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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