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Method for detecting plasticizer content in solid sample by headspace solid phase microextraction gas chromatography-tandem mass spectrometry

A technology of tandem mass spectrometry and gas chromatography, which is applied in the field of headspace solid-phase microextraction gas chromatography-tandem mass spectrometry in the detection of plasticizer content in solid samples, to achieve the effects of simple pretreatment, expanded range, and improved accuracy and efficiency

Inactive Publication Date: 2012-06-27
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

The combination of these two techniques applied to the detection of plasticizers has not been reported

Method used

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  • Method for detecting plasticizer content in solid sample by headspace solid phase microextraction gas chromatography-tandem mass spectrometry
  • Method for detecting plasticizer content in solid sample by headspace solid phase microextraction gas chromatography-tandem mass spectrometry
  • Method for detecting plasticizer content in solid sample by headspace solid phase microextraction gas chromatography-tandem mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1: Qualitative and quantitative analysis of plasticizers in the traditional Chinese medicine Xiaobupleurum granules

[0043] The operation steps are as follows:

[0044] Dilute the PAEs mixed standard solution (1000mg / L) into a series of concentrations: 100, 75, 50, 10, 5, 2, 1, 0.5mg / L, and dilute the PAEs isotope compound mixed solution (100mg / L) into 1.0-2.0mg / L internal standard solution. Take 1.0-2.0 μl of standard solution and internal standard solution for HS-SPME-GC-MS / MS experiment: heat the headspace bottle at 120-160°C for 15-25min, and use a static headspace solid-phase microextraction device ( 50 / 30μmDVB / CAR / PDMS Fiber) extraction for 5-15min, analysis at the inlet of 245-255℃ for 10-20min, and then GC-MS / MS analysis. The analysis results are shown in Table 1. At the same time, different collision energies are optimized, and appropriate collision energies are selected for different channels, as shown in the attached Figure 5 shown.

[0045] Ta...

Embodiment 2

[0053] Embodiment 2: Qualitative and quantitative analysis of plasticizer in coffee sample

[0054] The operation steps are as follows:

[0055] Dilute the PAEs mixed standard solution (1000mg / L) into a series of concentrations: 100, 75, 50, 10, 5, 2, 1, 0.5mg / L, and dilute the PAEs isotope compound mixed solution (100mg / L) into 1.0-2.0mg / L internal standard solution. Take 1-2 μl of standard solution and internal standard solution for HS-SPME-GC-MS / MS experiment: heat the headspace bottle at 120-160°C for 15-25min, use a static headspace solid-phase microextraction device (50 / 30μm DVB / CAR / PDMSFiber) extraction for 5-15min, analysis at the inlet of 245-255℃ for 10-20min, and then GC-MS / MS analysis. The analysis results are shown in Table 1. At the same time, different collision energies are optimized, and appropriate collision energies are selected for different channels, as shown in the attached Figure 5 shown.

[0056] Take 1.0-6.0g of sample coffee and put it into a 2...

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Abstract

The invention relates to a method for detecting the plasticizer content in a solid sample by headspace solid phase microextraction gas chromatography-tandem mass spectrometry, and the method combines an isotope internal standard and the headspace solid phase microextraction gas chromatography-tandem mass spectrometry (HS-SPME-GC-MS / MS) analysis for qualitative or quantitative analysis of a dimethyl phthalate plasticizer in a sample. The method mainly comprises the following steps of: a) mixing the solid sample with the isotope internal standard, and conducting extraction with headspace solid phase microextraction equipment; b) carrying out sample analysis; C) performing GC-MS / MS analysis; and d) implementing result treatment and quantitative analysis. The method of the invention is a fast, efficient, sensitive analysis method.

Description

technical field [0001] The invention relates to a method for discovering a solid sample by headspace solid phase microextraction gas chromatography-tandem mass spectrometry, and further refers to a method for discovering gas chromatography-tandem mass spectrometry (HS-SPME-GC-MS) using an isotope internal standard in combination with headspace solid phase microextraction / MS) analysis is a method for qualitative or quantitative analysis of dimethyl phthalate plasticizers in solid samples. Lay the groundwork and determine whether plasticizer levels in food and pharmaceuticals are safe and reliable. technical background [0002] Phthalates (PAEs) are widely used in the production of food packaging bags, plastic toys, textiles, cosmetics and other products due to their good performance and low cost. PAEs are added to the polymer as a plasticizer to interact with the secondary molecules of the polymer chain, thereby improving the elasticity of the polymer. Since this interacti...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 郭寅龙陆森森张立王昊阳张菁
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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