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Bonded phase chromatographic analysis method for detecting benzophenone and isopropyl diaryliodoniumsalt ketone compounds in printing and packaging materials

A technology of isopropylthioxanthone, printing and packaging, applied in the field of physical and chemical inspection

Active Publication Date: 2014-12-03
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned method using gas chromatography-mass spectrometry as the analytical instrument requires expensive high-purity helium as the mobile phase, and the inspection cost is high.

Method used

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  • Bonded phase chromatographic analysis method for detecting benzophenone and isopropyl diaryliodoniumsalt ketone compounds in printing and packaging materials
  • Bonded phase chromatographic analysis method for detecting benzophenone and isopropyl diaryliodoniumsalt ketone compounds in printing and packaging materials
  • Bonded phase chromatographic analysis method for detecting benzophenone and isopropyl diaryliodoniumsalt ketone compounds in printing and packaging materials

Examples

Experimental program
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Effect test

example 1

[0048] 1) Chromatographic conditions

[0049] Columns used are Acquity UPC 2 CSH Fluoro-Phenyl chromatographic column; the system back pressure is 1800 psi; the chromatographic column temperature is 50°C; the injection volume is 3 μL; the mobile phases are carbon dioxide (mobile phase A) and methanol (mobile phase B); the column flow rate is 1.5 mL / min; mobile phase gradient elution program as listed in Table 1 above. Monitoring was carried out at an ultraviolet wavelength of 246 nm.

[0050] 2) Preparation of standard solution

[0051] Accurately weigh 50 mg of various photoinitiators, accurate to 0.1 mg, dissolve them in acetonitrile and dilute them in 10 mL brown volumetric flasks to prepare a single standard stock solution with a concentration of 5 mg / mL. Then accurately pipette 1 mL of the single standard stock solution into a 50 mL brown volumetric flask, and dilute to the mark with acetonitrile to prepare a mixed standard solution with a concentration of 100 mg / L. ...

example 2

[0061] The six photoinitiators investigated in the experiment have the characteristics of similar structure, many isomers, and difficult to separate; in addition, UPC 2 There are many types of chromatographic columns used in the system, including normal-phase and reverse-phase LC chromatographic columns. Therefore, the experiment first investigates the influence of different stationary phase chromatographic columns on the separation. In this experiment, four chromatographic columns with significantly different stationary phases were selected for conditional screening, namely ACQUITY UPC 2 BEH, BEH 2-EP, HSS C18 SB, and CSH Fluoro-Phenyl. The experimental results show that (such as image 3 ), Acquity UPC 2 The CSH Fluoro-Phenyl chromatographic column can achieve the separation of these 6 compounds, which is related to the specific selectivity of the fluorophenyl stationary phase for the retention of the target. Therefore the chromatographic column that the final claim of ...

example 3

[0063] The present invention investigates the influence of different pressures (1600, 1800 and 2000 psi) and different chromatographic column temperatures (40, 50 and 60° C.) on the separation effect. The experimental results show that (such as Figure 4~5 ), with the increase of pressure and column temperature, the resolution of the 6 compounds increases, and the compound peaks are pushed back, but too high pressure will cause the pressure of the convergence chromatographic system to be too high, thus exceeding the instrument's own Pressure requirements, so the pressure required by the final claim of the present invention is 1800 psi; at the same time, too high temperature of the chromatographic column will cause the compound to peak slowly, so the temperature of the chromatographic column required by the final claim of the present invention is 50°C .

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Abstract

A bonded phase chromatographic analysis method for detecting benzophenone and isopropyl diaryliodoniumsalt ketone compounds in printing and packaging materials is characterized in that acetonitrile is used for extracting residual BP, 2-MBP, 3-MBP, 4-MBP, 2-ITX and 4-ITX in sample base materials, the extract liquor is separated through a bonded phase color spectrum and detected through an ultraviolet detector after being filtered through an organic phase filter membrane, and finally the contents of the six compounds in the printing and packaging materials can be finally detected. The method has the advantages that the method for analyzing the six compounds in the printing and packaging materials is set up through the bonded phase chromatography technology for the first time, the six analogue compounds or isomerides can be effectively separated and quantified in 2.5 minutes, a main mobile phase which is adopted is CO2, the consumption of organic solvents is extremely small, therefore, the method better conforms to the requirement for green and environmental protection analysis and detection, the cost is low, the sensitivity and the accuracy are high, and the repeatability is good.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical testing, specifically a method for detecting benzophenone, 2-methylbenzophenone, 3-methylbenzophenone, 4-methylbenzophenone, Convergence chromatography analysis method for 2-isopropylthioxanthone and 4-isopropylthioxanthone compounds. Background technique [0002] Benzophenone (BP), methylbenzophenone (MBP) and isopropylthioxanthone (ITX) are important ultraviolet (UV) absorbers and initiators that are widely used in UV inks. The results of toxicology tests recently completed by Rhodes et al. showed that BP not only has carcinogenic effects on experimental animals, but also has skin contact toxicity and reproductive toxicity. In 2011, Germany announced the recall of frozen thin noodles imported from Belgium. The main reason was that the BP contained in the printing ink on the noodle packaging penetrated into the noodles, causing the noodles to be contaminated. The detected BP conten...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 李中皓唐纲岭范子彦陈再根边照阳吴帅宾罗彦波杨飞刘珊珊刘洋
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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