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Co-detection determination method of residual quantity of preservative and antioxidant in water-based adhesive

A determination method and technology of water-based glue, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of simultaneous analysis and accurate quantification of affected substances, uneven dispersion of emulsion liquid chromatography, and inability to separate peaks clearly. The effect of correlation, short detection time and high sensitivity

Active Publication Date: 2016-04-27
CHINA TOBACCO YUNNAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ultrasonic treatment will cause water-based glue and extract to form a turbid emulsion, and the emulsion is not suitable for liquid chromatography due to uneven dispersion
Rising temperature will cause a large amount of other substances in the water-based glue to be extracted into the extract, forming too many interference peaks, resulting in the peaks of the components to be measured cannot be clearly separated, causing difficulties in the selection of subsequent chromatographic conditions, and affecting the above-mentioned substances. Simultaneous analysis and accurate quantification of

Method used

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  • Co-detection determination method of residual quantity of preservative and antioxidant in water-based adhesive
  • Co-detection determination method of residual quantity of preservative and antioxidant in water-based adhesive
  • Co-detection determination method of residual quantity of preservative and antioxidant in water-based adhesive

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The present embodiment is as follows to the assay method of MI, CMI, BIT and BHT residual amount in the commercially available water-based glue sample:

[0029] (1) Preparation of standard solution: Accurately weigh 50 mg of 2-methyl-3(2H)-isothiazolinone (MI), 5-chloro-2-methyl-2H-isothiazol-3-one (CMI) 100mg, 50mg of 1,2-benzisothiazolyl-3(2H)-one (BIT) and 10mg of 2,6-di-tert-butyl-4-methylphenol (BHT) were respectively placed in a 100mL brown volumetric flask, Add methanol to dissolve under ultrasonic conditions and dilute to the mark, shake well, and prepare standard stock solution. Store the stock solution in the refrigerator. Pipette the quasi-stock solution, and prepare 2-methyl-3(2H)-isothiazolinone (MI) concentrations of 0.5, 2.5, 5.0, 25.0, 50.0 μg / mL, and 5-chloro -2-Methyl-2H-isothiazol-3-one (CMI) concentration is 1.0, 5.0, 10.0, 50.0, 100.0μg / mL, 1,2-benzisothiazolyl-3(2H)-one (BIT ) concentrations of 0.5, 2.5, 5.0, 25.0, 50.0 μg / mL, and 2,6-di-tert-bu...

Embodiment 2

[0046] The present embodiment is as follows to the detection method of the repeatability of the inventive method and the standard addition recovery rate:

[0047] Select sample 6 and sample 10 as the background, adopt the sample addition standard recovery rate test, add MI, CMI, BIT and BHT standard solution to the background, carry out the addition recovery test, add three different concentrations of low, medium and high, each Each concentration was repeatedly measured 5 times, and the chromatographic analysis conditions were the same as in Example 1. According to the analysis results, the recovery rate of standard addition of MI, CMI, BIT and BHT in the water-based glue of this method and the relative standard deviation of the measured value after the standard addition were calculated. The results are as follows: Table 3 shows.

[0048] The standard recovery rate test result (n=5) of this method of table 3

[0049]

[0050] It can be seen from Table 3 that the recovery r...

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Abstract

The invention discloses a co-detection determination method of residual quantity of a preservative and an antioxidant in a water-based adhesive. The method of the invention comprises steps as follows: preparation of a sample solution, high performance liquid chromatography, calculation of determination results and the like. The co-detection determination method has advantages of short detection time, simple operation, high sensitivity, high recovery rate, good repeatability and the like. Under chromatographic conditions in the method, separation of chromatographic peaks of MI, CMI, BIT and BHT from chromatographic peaks of impurities is good, and correlation is good. Limits of detection are respectively 0.065, 0.121, 0.046 and 0.052 microgram / mL. The average recovery of standard addition at low-medium-high three addition levels is within 88.7-93.8%. The average relative standard deviation of sample determination results is less than 5%. It shows that the method has high recovery rate and good repeatability. The invention provides scientific basis for quality surveillance of the water-based adhesive.

Description

technical field [0001] The invention relates to the technical field of preservatives and antioxidants, in particular to a method for co-detection and determination of residual amounts of preservatives and antioxidants in water-based adhesives. Background technique [0002] Water-based adhesives are mainly used in various packaging and printing, wood processing, construction and other industries. In order to prolong the shelf life and service life of water-based adhesives, isothiazolinone preservatives and phenolic antioxidants are used in the production of water-based adhesives. Some processing aids are often added during the manufacturing process. [0003] Isothiazolinone and its derivatives are a very important class of heterocyclic compounds in bactericidal preservatives, which can be used in almost all fields that need to kill microorganisms except for sanitation and food fields. In recent years, the production and application of isothiazolinone fungicides in my country...

Claims

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Application Information

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IPC IPC(8): G01N30/06
Inventor 陈建华缪恩铭李雪梅徐济仓魏玉玲耿永勤李晶杨叶昆黄海涛
Owner CHINA TOBACCO YUNNAN IND
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