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Method for measuring three isothiazolinone preservatives in cigarette paper by liquid chromatography-tandem mass spectrometry

A liquid chromatography and isothiazoline technology, applied in the field of three kinds of isothiazolinone preservatives, can solve the problems of strong allergens, skin irritation, allergies, etc., and achieve the effect of fast operation, improved precision and stable response

Inactive Publication Date: 2018-01-05
CHINA TOBACCO ZHEJIANG IND
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Problems solved by technology

Isothiazolinone compounds are commonly used fungicides, but such compounds, especially 5-chloro-2-methyl-isothiazolin-3-one (CMI) and 2-methyl-4-isothiazoline- 3-ketone (MI) is a skin irritant and a strong allergen, and may cause allergies even in the specified concentration range

Method used

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  • Method for measuring three isothiazolinone preservatives in cigarette paper by liquid chromatography-tandem mass spectrometry
  • Method for measuring three isothiazolinone preservatives in cigarette paper by liquid chromatography-tandem mass spectrometry
  • Method for measuring three isothiazolinone preservatives in cigarette paper by liquid chromatography-tandem mass spectrometry

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Embodiment

[0036] (1) Reagents and instruments

[0037] Reagents: Methanol and formic acid are chromatographically pure and ultrapure water. 1,2-Benzisothiazolyl-3(2H)-one-13C6 (BIT-13C6) (purity ≥ 98.0%, Canada Tornoto Research Chemical Company), 2-methyl-4-isothiazolin-3-one (MI), 5-chloro-2-methyl-isothiazolin-3-one (CMI), 1,2-benzisothiazolyl-3(2H)-one (BIT) (purity ≥ 98.0%, Germany Dr. Ehrenstorfer Company).

[0038]Instruments: Thermo Scientific TSQ Quantum Ultra triple quadrupole mass spectrometer, ThermoScientific Surveyor Plus high-performance liquid chromatography system (Thermo Fisher, USA); KQ500-DB ultrasonic generator (Jiangsu Kunshan Ultrasonic Instrument Co., Ltd.); TSQ-280 constant temperature oscillator (Shanghai Jinghong Experimental Equipment Co., Ltd.); XP205 electronic balance (sensitivity: 0.0001 g, Mettler-Toledo, Switzerland); CORTECS C18+ chromatographic column (2.1mm×100mm, 2.7μm, Waters, USA); Milli-Q ultrapure Water system (Millipore, USA).

[0039] (2) P...

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Abstract

The invention discloses a method for measuring three isothiazolinone preservatives in cigarette paper by liquid chromatography-tandem mass spectrometry, comprising the following steps: (1) preparing amixed standard solution containing three isothiazolinones, and carrying out quantitative analysis by an internal standard method to obtain a standard curve linear regression equation; (2) cutting a sample into a square with side length being 0.4-0.6 cm, weighing and taking cigarette paper to be measured into an Erlenmeyer flask, adding water and an internal standard solution, carrying out ultrasonic extraction, and filtering through a 0.22-micron water-phase filter membrane to obtain a sample solution to be measured; and (3) analyzing the sample solution to be measured by liquid chromatography-tandem mass spectrometry, and respectively calculating according to the standard curve linear regression equation so as to obtain concentrations of the three isothiazolinones. The analytic method for simultaneously measuring contents of three isothiazolinones in cigarette paper is fast to operate, is simple and feasible, has advantages of stable response, environmental solvent and high extraction efficiency, and can avoid liquid chromatographic solvent effect caused by methanol extraction and sample introduction.

Description

technical field [0001] The invention relates to the field of cigarette paper, in particular to a method for measuring three kinds of isothiazolinone preservatives in cigarette paper by liquid chromatography-tandem mass spectrometry. 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 and other fields . [0003] In the paper industry, the temperature during production is generally maintained at about 30°C. Such production conditions promote the growth and reproduction of microorganisms. Microbial pollution sources can reduce the physical properties of pulp, can make a variety of additives ineffective, and cause varying degrees of impact on papermaking equipment. Therefore, fungicides are usually added in the papermaking process to inhibit micro...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/14G01N30/16G01N30/34
Inventor 卢昕博戴路周国俊肖卫强杨君王雨凝斯文徐建史春云尹洁刘金莉
Owner CHINA TOBACCO ZHEJIANG IND
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