Quantitative determination method for methylisothiazolinone and chloro methyl isothiazolinone in water-based adhesive

A technology of methylisothiazolinone and methylchloroisothiazolinone is applied in the field of quantitative determination of methylisothiazolinone and its chlorinated methylchloroisothiazolinone in water-based glue, and can solve the problem of unsolved problems. See the literature reports of MI and CMI detection, etc., to achieve the effect of simple operation, fast analysis speed, good accuracy and stability

Active Publication Date: 2014-01-01
CHINA TOBACCO GUANGXI IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] [3] Currently reported detection methods for MI and CMI mainly detect toys, water, food packaging paper, etc., and there are no literature reports on the detection of MI and CMI in water-based adhesives

Method used

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  • Quantitative determination method for methylisothiazolinone and chloro methyl isothiazolinone in water-based adhesive
  • Quantitative determination method for methylisothiazolinone and chloro methyl isothiazolinone in water-based adhesive
  • Quantitative determination method for methylisothiazolinone and chloro methyl isothiazolinone in water-based adhesive

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Embodiment Construction

[0014] The following implementation process and examples are intended to further illustrate the present invention and should not be regarded as limiting the present invention.

[0015] [1] Pre-processing method:

[0016] Weigh 1.000g of the water-based glue sample into a 50mL Erlenmeyer flask with a stopper, add 15mL of methanol, mix well, and extract with ultrasonic frequency 40KHz for 20min. Take about 10mL of the solution in a centrifuge tube and centrifuge at 12000g for 10min. The supernatant after centrifugation is filtered through a 0.45μm organic phase filter membrane and analyzed by liquid chromatography.

[0017] [2] Liquid chromatography analysis conditions:

[0018] Chromatographic column: C18 column (5μm, 250mm×4.6mm, Agilent); mobile phase: A: water; B: methanol; mobile phase methanol: water = 50:50, flow rate: 0.8mL / min; column temperature 30°C; Injection volume: 10 μL. The retention time was compared with the standard sample for qualitative analysis, and the ...

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Abstract

The invention discloses a quantitative determination method for methylisothiazolinone (MI) and chloro methyl isothiazolinone (CMI) in a water-based adhesive by utilizing a high-performance liquid chromatographic instrument. The method comprises the following steps: under the supersonic frequency of 30-40 KHz, using methanol as an extraction solution, and extracting the MI and CMI in the water-based adhesive for 15-60 min; using a C18 chromatographic column as an analysis column, using a methanol and water mixed solution as a mobile phase, and utilizing the high-performance liquid chromatographic instrument with an ultraviolet detector to determine the content of the MI and CMI in the water-based adhesive. The quantitative determination method has the characteristics of simplicity and convenience in operation, quick analysis, high sensitivity, and high accuracy and stability, and is particularly suitable for the analysis of MI and CMI in a large amount of the water-based adhesive.

Description

technical field [0001] The invention relates to the technical field of bactericidal preservatives, in particular to a quantitative determination method for methylisothiazolinone and its chlorinated product methylchloroisothiazolinone in water-based glue. Background technique [0002] [1] Methylisothiazolinone (MI), chemical name is 2-methyl-4-isothiazolin-3-one; Methylchloroisothiazolinone (CMI), chemical name is 5-chloro-2 -Methyl-4-isothiazolin-3-one, belonging to isothiazolinone and its derivatives, is a new type of high-efficiency broad-spectrum fungicide, widely used in cosmetics, coatings and other industries for antiseptic sterilization. Isothiazolinone compounds not only cause sensitization to the skin, but also cause skin burns or asthma in addition to symptoms such as eye and skin contact allergies or dermatitis. Among them, MI and CMI are the most sensitizing isothiazolines Ketone derivatives can be sensitized at the first contact and are strong allergens. Water...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 周晓李小兰陈志燕孟冬玲周芸朱静
Owner CHINA TOBACCO GUANGXI IND
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