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Multi-component substance high performance liquid detection and analysis method

An analytical method and high-performance liquid phase technology, applied in the fields of detection and chemical analysis and detection, can solve the problems of high purchase cost of equipment, cumbersome work, few types of detection, analysis and detection, etc. Check the effect of analysis results

Pending Publication Date: 2020-06-16
SICHUAN HUIYU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, when using infrared spectroscopy and ultraviolet spectroscopy to detect antioxidants, the specificity of the detection method is poor, and the interference of the sample matrix is ​​obvious, and it is impossible to detect multiple antioxidants at the same time; the detection sensitivity is low and cannot meet the requirements of the current stage. Relevant guidelines for the control of the limits of antioxidants
Gas chromatography-mass spectrometry GC-MS, ultra-high performance liquid chromatography UPLC, and liquid chromatography-mass spectrometry LC-MS require special detection equipment, and the purchase cost of equipment is high. Ordinary laboratories cannot perform detection, and need to entrust a third-party organization for detection, which is expensive.
Ordinary high-performance liquid chromatography has low detection efficiency, and there are few types of detection and analysis for each detection. For the quality analysis of COP plastic bottles containing more than 10 antioxidant components, the work is cumbersome and inefficient

Method used

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  • Multi-component substance high performance liquid detection and analysis method
  • Multi-component substance high performance liquid detection and analysis method
  • Multi-component substance high performance liquid detection and analysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Preparation of the test solution

[0045] Accurately weigh 6.25 mg each of the 14 substances in Table 1, dissolve and dilute with methanol to a solution with a concentration of 0.25 μg / ml to obtain the test solution.

[0046] (2) need testing solution is crossed reversed-phase liquid phase chromatographic column and is separated and analyzed;

[0047] Chromatographic conditions:

[0048] Detection wavelength: 220nm

[0049] Flow rate: 1.0ml / min

[0050] Column temperature: 40°C

[0051] Injection volume: 20μl

[0052] Chromatographic column: Agilent InfinityLab poroshell 120EC-C18 150m×4.6mm 4μm

[0053] Mobile phase A: methanol-water-phosphoric acid

[0054] Mobile Phase B: Methanol

[0055] In mobile phase A, methanol, water and phosphoric acid were mixed in a volume ratio of 500:500:0.4. The phosphoric acid is an 85% aqueous phosphoric acid solution by volume.

[0056] Carry out gradient elution according to the following table:

[0057]

[0058] The...

Embodiment 2

[0064] The difference between Example 2 and Example 1 is that in the mobile phase A of Example 2, methanol, water and phosphoric acid are mixed in a volume ratio of 450:550:0.6. And embodiment 2 carries out gradient elution according to the table:

[0065]

[0066] The experimental detection results of Example 2 are shown in Table 3.

[0067] table 3

[0068]

[0069] The detection result chromatogram of embodiment 2 is as Figure 4 Shown (27.670 is the detection peak of S element, which is not within the statistical range of this experiment). From Table 3 and Figure 4 It can be seen that, with the detection and analysis method of Example 2, except for the resolution between Irgafos126 and Irgafos168oxide which is 1.26, the minimum resolution among other components is greater than 2, and the peak shape of each component is good.

Embodiment 3

[0071] The difference between Example 3 and Example 1 is that the mobile phase A of Example 3 does not contain phosphoric acid, that is, in the mobile phase A of Example 3, methanol and water are mixed at a volume ratio of 500:500. The experimental detection results of Example 3 are shown in Table 4.

[0072] Table 4

[0073]

[0074] The detection result chromatogram of embodiment 3 is as Figure 5 (27.433 is the detection peak of S element, which is not within the statistical range of this experiment). From Table 4 and Figure 5 It can be seen that the detection and analysis method of Example 3 has a minimum resolution of 1.64 among the components, and the resolution is greater than 1.5. Except for Fenoksan, the peak shapes of the chromatograms of other components are all good.

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Abstract

The invention discloses a multi-component substance high performance liquid detection and analysis method, which belongs to the technical field of chemical analysis and detection. The method comprisessteps of preparing a test solution, enabling the test solution to pass through a reversed-phase liquid chromatographic column for separation and analysis, and filling the reversed-phase liquid chromatographic column with silica gel chromatographic column filler particles with a solid core-shell structure. The process structure of the chromatographic silica gel column is improved, with the matching of the mobile phase design and the chromatographic analysis mobile phase gradient program improvement, the 14 phenolic antioxidant components in the COP bottle can be simultaneously detected so as to obtain the chromatogram, such that the related impurity separation degree is high, the peak shape is good, and the analysis detection efficiency and the detection result accuracy are substantially improved.

Description

technical field [0001] The invention relates to a detection method, in particular to a high-efficiency liquid phase detection and analysis method for multi-component substances, which belongs to the technical field of chemical analysis and detection. Background technique [0002] As an indispensable auxiliary material in the plastic industry, antioxidants are used to reduce the oxidation rate of plastic materials, delay the aging phenomenon, and prolong the life of plastic products. Among them, phenolic antioxidants are the most widely used and most used oxidants in plastics. They have the characteristics of good antioxidant effect, good compatibility and high thermal stability. They are widely used in polyethylene, polypropylene and various rubber products. In recent years, the United States Food and Drug Administration (FDA), the European Commission (EC) and my country have carried out theoretical and experimental research results on the migration of packaging materials ch...

Claims

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Application Information

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IPC IPC(8): G01N30/89G01N30/06G01N30/60G01N30/56
CPCG01N30/89G01N30/06G01N30/6052G01N30/56G01N2030/562
Inventor 李彬杨玉容胡和平
Owner SICHUAN HUIYU PHARMA