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Method for detecting dibutyl sebacate and acetyl tributyl citrate in film material

A technology of acetyl tributyl citrate and dibutyl sebacate, which is applied in the field of detection of dibutyl sebacate and acetyl tributyl citrate in membrane materials, can solve the problems of few reports and literature, Achieve the effect of simple operation, high economic and social value, and high sensitivity

Pending Publication Date: 2019-05-21
SHANDONG INST FOR PROD QUALITY INSPECTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the detection methods of dibutyl sebacate and acetyl tributyl citrate in food packaging materials have not been formulated in our country's standards, and there are few reports and literature

Method used

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  • Method for detecting dibutyl sebacate and acetyl tributyl citrate in film material
  • Method for detecting dibutyl sebacate and acetyl tributyl citrate in film material
  • Method for detecting dibutyl sebacate and acetyl tributyl citrate in film material

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Experimental program
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Effect test

Embodiment 1

[0039] 1.1 Reagents, standards and materials

[0040] Methanol, n-hexane, dichloromethane: chromatographically pure, Merck; dibutyl sebacate, chemical substance registration number (CAS): 109-43-3, purity 99.4%, Shanghai Anpu Experiment Technology Co., Ltd. Acetyl tributyl citrate: CAS: 77-90-7, purity 98%, Shanghai Anpu Experimental Technology Co., Ltd.; organic filter membrane: pore size 0.45 μm, Tianjin Keyilong Experimental Equipment Co., Ltd. PVDC film was used as the test sample.

[0041] 1.2 Sample preparation

[0042] Select 3 PVDC film samples and 3 PVDC composite film samples as test samples, and detect and analyze the dibutyl sebacate and acetyl tributyl citrate contained in the samples. The sample number is 1 # ,2 # 、3 # 、4 # 、5 # 、6 # .

[0043] Weigh 5.0g of sample, cut or pulverize the sample into individual fragments, the particle size should be ≤0.2cm, mix evenly; do blank test at the same time.

[0044] Accurately weigh 0.20g (accurate to 0.1mg) of t...

Embodiment 2

[0049] 2.1 Selection of chromatographic column

[0050] Capillary column: TR-FFAP type chromatographic column (30m×0.32mm×0.25μm) strong polar chromatographic column, the polar stationary phase is polyethylene glycol, the response value of the two target substances is too low during separation, and the separation effect is not good. In addition, the boiling points of dibutyl sebacate and acetyl tributyl citrate are 178°C and 343°C respectively, and the maximum tolerance temperature of the TR-FFAP column is 250°C. not good, such as figure 1 shown. The DB-1 type capillary column (30m×0.25mm×0.50μm) has a poor separation effect on acetyl tributyl citrate, such as figure 2 shown. DB-5MS type capillary column (30m×0.25mm×0.25μm) has good separation effect and good peak shape. Since the maximum temperature tolerance is 350°C, the column loss is very low, and it is inert to active compounds. It has higher sensitivity and mass spectrometry Figure integrity, is an ideal non-polar ...

Embodiment 3

[0068] a. Chromatographic conditions

[0069] Chromatographic column: DB-5MS quartz capillary column (30m×0.25mm×0.25μm); heating program: initial column temperature is 60°C, keep it for 1min, raise the temperature to 220°C at 20°C / min, keep it for 1min, then increase the temperature at 5°C / min The temperature was raised to 280°C and kept for 5 minutes, the flow rate of carrier gas (He) was 1mL / min, the sampling method was splitless injection, and the injection volume was 1.0 μL. Injection port temperature: 280°C.

[0070] b. Mass Spectrometry Conditions

[0071] Electron impact (EI) ion source; electron energy: 70eV; ion source temperature: 230°C; transfer line temperature: 280°C; quadrupole temperature: 150°C; solvent delay time: 5min; monitoring method: selected ion scanning mode (SIM) . See Table 5 for the quantitative and qualitative ions of dibutyl sebacate and acetyl tributyl citrate.

[0072] Table 5 Fragment ion information of dibutyl sebacate and acetyl tributyl ...

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Abstract

The invention relates to the technical field of chemical substance detection, in particular to a method for detecting dibutyl sebacate and acetyl tributyl citrate in a film material. The method comprises: weighing a to-be-detected film material and carrying out extraction by using an organic solvent to obtain an extracting solution; and detecting the extracting solution by using gas chromatography-mass spectrometer. The method is operated simply and easily; the result is accurate and reliable; the potential safety hazard in the film material can be discovered timely to realize an early warningeffect; and a technical support is provided for the risk monitoring of membrane material packaging products in China. The method has the broad application prospects and great economic and social values.

Description

technical field [0001] The invention relates to the technical field of chemical substance detection, in particular to a method for detecting dibutyl sebacate and acetyl tributyl citrate in membrane materials. Background technique [0002] Polyvinylidene chloride (PVDC) has excellent properties such as high barrier properties, high strength and toughness, high transparency, good heat sealing and maintaining food flavor, and is widely used in many fields, especially in the food plastic packaging industry. Due to the good oxygen and moisture permeability of PVDC materials, especially in the aspect of odor barrier, it is mainly used in the packaging of meat products, dairy products, pastries and other products. Its good barrier properties not only prolong the shelf life of food, And improve its economic value. In the production of PVDC materials, in order to enhance the corresponding performance, manufacturers usually add additives such as epoxy soybean oil, dibutyl sebacate an...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/72
Inventor 张智力王微山杨学军
Owner SHANDONG INST FOR PROD QUALITY INSPECTION
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