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UPC<2> (ultra performance convergence chromatographic) analysis method for detecting DEAB and MK in printing and packaging material

An ultra-efficient confluence, printing and packaging technology, applied in the field of physical and chemical inspection

Active Publication Date: 2014-01-08
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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  • UPC&lt;2&gt; (ultra performance convergence chromatographic) analysis method for detecting DEAB and MK in printing and packaging material
  • UPC&lt;2&gt; (ultra performance convergence chromatographic) analysis method for detecting DEAB and MK in printing and packaging material
  • UPC&lt;2&gt; (ultra performance convergence chromatographic) analysis method for detecting DEAB and MK in printing and packaging material

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0050] 1) Chromatographic conditions

[0051] 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 348 nm.

[0052] 2) Preparation of standard solution

[0053] 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

[0063] UPCs 2 There are many types of chromatographic columns used in the system, including normal-phase and reverse-phase liquid chromatography (LC) chromatographic columns. Therefore, the present invention first investigates the influence of different chromatographic columns on separation. In this experiment, 4 chromatographic columns with obvious differences were selected for conditional screening, namely ACQUITY UPC 2 BEH, ACQUITY UPC 2 BEH 2-EP, ACQUITY UPC 2 HSS C18 SB and ACQUITY UPC 2 CSH Fluoro-Phenyl. From the experimental results ( figure 2 ) It can be seen that the four chromatographic columns can achieve good separation effects for these two substances, and the retention capabilities of the four chromatographic columns for DEAB and MK are: CSH Fluoro-Phenyl>HSS C18 SB> BEH 2-EP > BEH. Therefore, the chromatographic column claimed in the final claim of the present invention can be one of the four chromatographic columns.

[0064]

example 3

[0066] The present invention investigates the influence of different pressures (1600 psi, 1800 psi and 2000 psi) and different chromatographic column temperatures (40°C, 50°C and 60°C) on the separation effect. The experimental results show that (such as Figure 3~4 ), the two compounds can be well separated under the experimental temperature and pressure. However, too high pressure will cause the pressure of the convergence chromatography system to rise, thereby exceeding the pressure resistance requirements of the instrument itself. Therefore, the temperature of the chromatographic column required by the final claim of the present invention is 40-60° C., and the column pressure is 1600-1800 psi.

[0067]

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Abstract

The invention discloses a UPC<2> (ultra performance convergence chromatographic) analysis method for detecting DEAB and MK in a printing and packaging material. The method is characterized by comprising the following steps of extracting remaining DEAB and remaining MK in a sample substrate by using acetonitrile, performing separation by using UPC<2> after extraction liquid is filtered by an organic phase filter membrane, and performing detection by using an ultraviolet detector to finally determine the DEAB content and the MK content of a printing and packaging material sample. The method has the effects that a UPC<2> technology is used for the first time, an analysis method for the DEAB and the MK in the printing and packaging material is established, two similar compounds can be effectively separated and quantified within 4 minutes by the analysis method, and compared with a conventional common analysis method, the analysis method has the advantage that the detection time is remarkably shortened; carbon dioxide is adopted as a main flowing phase, and the consumption of an organic solvent is extremely low, so that the requirements of environment-friendly analysis and detection are better met; a gas flowing phase with lower cost is adopted, and meanwhile, the analysis time is short, so that the detection and analysis cost is greatly lowered; the method is high in sensitivity, accuracy and repeatability.

Description

[0001] technical field [0002] The invention belongs to the technical field of physical and chemical testing, in particular to 4,4-bis(diethylamino)benzophenone (DEAB) and 4,4-bis(dimethylamino)benzophenone (MK ) ultra-high performance convergence chromatography analysis method. Background technique [0003] 4,4-bis(diethylamino)benzophenone (DEAB) and 4,4-bis(dimethylamino)benzophenone (MK) are important ultraviolet (UV) absorbers and initiators, in UV It is widely used in ink, and it is also one of the important pollutant indicators of deinking recycled fiber recycled paper. In 2007, the European Union explicitly banned the use of DEAB and MK in printing inks for food contact materials in the Res AP (2002) Resolution 1 of some member states on "Paper and paperboard materials and products intended to come into contact with food". [1] . [0004] Ultra performance convergence chromatography (UPC) 2 ) [2] technology is a recently proposed separation technology, which or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 李中皓吴帅宾罗彦波唐纲岭范子彦杨飞刘珊珊边照阳陈再根陈欢
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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