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Method for determining three types of isothiazolinone preservatives in water-based glue by adopting liquid chromatography-tandem mass spectrum

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 effects of fast operation, good repeatability and simple operation

Active Publication Date: 2015-04-29
CHINA TOBACCO ZHEJIANG IND
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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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  • Method for determining three types of isothiazolinone preservatives in water-based glue by adopting liquid chromatography-tandem mass spectrum
  • Method for determining three types of isothiazolinone preservatives in water-based glue by adopting liquid chromatography-tandem mass spectrum
  • Method for determining three types of isothiazolinone preservatives in water-based glue by adopting liquid chromatography-tandem mass spectrum

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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: Thermo Scientific TSQ Quantum Ultra triple quadrupole mass spectrometer, Thermo Scientific Surveyor Plus high-performance liquid chromatography system (Thermo Fisher, USA); CORTECS C18+ chromatographic column (2.1 mm × 100 mm, 2.7 μm, 90?, Waters, USA ); Sigma 4-16K high-speed centrifuge (Sigma, Germany); KQ500-DB ultrasonic generator (Jiangsu Kunshan Ultrasonic Instrument Co., Ltd.); Milli-Q ultrapure water system (Millipore, USA); XP205 electronic balance (sensitivity: 0.0001 g, 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 ) (purity ≥ 98.0%, Tornoto R...

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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 testing of water-based glue, in particular to a liquid chromatography-tandem mass spectrometry method for the determination of three isothiazolinone preservatives in water-based glue. Background technique [0002] Isothiazolinone compounds are a class of high-efficiency, 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 a water-containing latex formed by emulsion polymerization. It is susceptible to microbial attack and chemical bond fracture, resulting in decreased viscosity, reduced adhesion, and delamination. In severe cases, it will deteriorate during the manufacture, transportation, and storage of the emulsion. Adding isothiazolinone to water-based glue can play a role in sterilization and antisepti...

Claims

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Application Information

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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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