A method for the determination of three isothiazolinone preservatives in water-based glue by liquid chromatography-tandem mass spectrometry

A technology of isothiazolinone and tandem mass spectrometry, which is applied in the field of physical and chemical inspection of water-based adhesives, and achieves the effect of fast operation, simple operation and high sensitivity

Active Publication Date: 2016-01-27
CHINA TOBACCO ZHEJIANG IND
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

At present, there is no report on the determination of isothiazolinone compounds in water-based glue by LC-MS / MS

Method used

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  • A method for the determination of three isothiazolinone preservatives in water-based glue by liquid chromatography-tandem mass spectrometry
  • A method for the determination of three isothiazolinone preservatives in water-based glue by liquid chromatography-tandem mass spectrometry
  • A method for the determination of three isothiazolinone preservatives in water-based glue by liquid chromatography-tandem mass spectrometry

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Embodiment Construction

[0018] The present invention is further described by the following specific examples, but does not limit the present invention.

[0019] 1. Instruments and reagents

[0020] Instruments: ThermoScientificTSQQuantumUltra triple quadrupole mass spectrometer, ThermoScientificSurveyorPlus high performance liquid chromatography system (ThermoFisher company in the United States); CORTECSC18+ chromatographic column (2.1mm×100mm, 2.7μm, American Waters company); Sigma4-16K high-speed centrifuge (German Sigma company); KQ500-DB ultrasonic generator (Jiangsu Kunshan Ultrasonic Instrument Co., Ltd.); Milli-Q ultrapure water system (U.S. Millipore company); XP205 electronic balance (sensing Quantity: 0.0001g, Mettler-Toledo, Switzerland).

[0021] Reagents: 2-methyl-4-isothiazolin-3-one (MI), 5-chloro-2-methyl-isothiazolin-3-one (CMI), 1,2-benzisothiazolyl- 3(2H)-ketone (BIT) (purity ≥98.0%, Dr.Ehrenstorfer, Germany), internal standard 1,2-benzisothiazolyl-3(2H)-one- 13 C 6 (BIT- 13 C 6 ) (Puri...

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Abstract

The invention relates to the technical field of physical and chemical inspection of water-based glue and particularly relates to a method for determining three types of isothiazolinone preservatives in water-based glue by adopting a liquid chromatography-tandem mass spectrum. A water-based glue sample is extracted with water and centrifuged, then is subjected to LC-MS / MS analysis and is quantified by an internal standard method. The concentration range of 2-methyl-4-isothiazolin-3-ketone (MI) and 5-chloro-2-methyl-isothiazolin-3-ketone (CMI) is 2.5ng / mL-250ng / mL, the concentration range of 1,2-benzisothiazol-3(2H)-ketone (BIT) is 5ng / mL-500ng / mL, the linear relation is good (R2 is more than or equal to 0.9996), the adding standard recovery rates of three adding levels are 96.3%-109.6%, the average relative standard deviation (RSD) is 1.5%-6.7%, and the limit of detection (LOD) and the limit of quantification (LOQ) of the method are 0.011mg / kg-0.015mg / kg and 0.035mg / kg-0.051mg / kg. The method is simple to operate, has high sensitivity and good repeatability, and is suitable for rapidly determining MI, CMI and BIT in the water-based glue.

Description

Technical field [0001] The invention relates to the technical field of physical and chemical inspection of water-based glue, and specifically relates to a method for determining three isothiazolinone preservatives in water-based glue by using liquid chromatography-tandem mass spectrometry. Background technique [0002] Isothiazolinone compounds are a kind of high-efficiency and broad-spectrum preservatives, which have good killing effects on bacteria, fungi, algae, etc., and are widely used in industrial circulating cooling water, adhesives, textiles, coatings, papermaking, etc field. Water-based glue is an aqueous latex formed by emulsion polymerization, which is susceptible to microbial attack and chemical bond breakage, resulting in decreased viscosity, decreased adhesion, and delamination. In severe cases, the emulsion will spoil and deteriorate during the manufacturing, transportation and storage of the emulsion. Adding isothiazolinone to water-based glue can play a role of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 卢昕博周国俊肖卫强许高燕史春云蒋健
Owner CHINA TOBACCO ZHEJIANG IND
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