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Method for detecting phthalate in tobacco essence or water-based adhesive

A technology for phthalates and tobacco flavors, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult to meet the detection requirements of phthalates in flavors, poor selectivity of single quadrupole mass spectrometer, High quantitation limit and other problems, to achieve the effect of simple pre-treatment method, strong anti-matrix interference ability, and purification of samples

Active Publication Date: 2020-03-17
CHINA TOBACCO GUANGXI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the matrix of fragrance samples is more complex than that of textiles and dairy products, many of which are natural extracts, the selectivity of single quadrupole mass spectrometry is poor and the limit of quantification is high, which is difficult to meet the detection requirements of phthalates in fragrances

Method used

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  • Method for detecting phthalate in tobacco essence or water-based adhesive
  • Method for detecting phthalate in tobacco essence or water-based adhesive
  • Method for detecting phthalate in tobacco essence or water-based adhesive

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0045] 1. Apparatus and reagents:

[0046] 13 kinds of phthalates and methanol are all chromatographic grade reagents; they meet the requirements of first grade water in GB / T 6682.

[0047] Agilent gas chromatography-tandem mass spectrometer; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g).

[0048] 2. Sample processing:

[0049] Weigh 0.2g of tobacco flavor sample (accurate to 0.01g) and place it in a 15mL Erlenmeyer flask with stopper. Accurately add 10 mL of ethanol, vortex and extract for 5 minutes; after centrifugation at 8000 rpm for 3 minutes, draw 2 mL of the filtrate and blow dry with nitrogen, reconstitute it with 2.0 mL of ultrapure water, and add 20 mg of magnetic graphene particles to the centrifuge tube at 2000 r / min Vortex for 3 minutes, and separate the solid and liquid phases with a magnet. Discard the water layer, add 1 mL of methanol, sonicate for 2 min, transfer the supernatant to a chromatographic bottle after magnetic separation, repeat the eluti...

example 2

[0055] According to the method described in Example 1, when another tobacco flavor sample was selected, the above 13 phthalates were not detected.

example 3

[0057] 1. Apparatus and reagents:

[0058] 13 kinds of phthalates and methanol are all chromatographic grade reagents; they meet the requirements of first grade water in GB / T 6682.

[0059] Agilent gas chromatography-tandem mass spectrometer; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g).

[0060] 2. Sample processing:

[0061] Weigh 0.2g sample of cigarette water-based gum (accurate to 0.01g) and place it in a 15mL Erlenmeyer flask with stopper. Accurately add 10 mL of ethanol, vortex and extract for 5 minutes; after centrifugation at 8000 rpm for 3 minutes, draw 2 mL of the filtrate and blow dry with nitrogen, reconstitute it with 2.0 mL of ultrapure water, and add 20 mg of magnetic graphene particles to the centrifuge tube at 2000 r / min Vortex for 3 minutes, and separate the solid and liquid phases with a magnet. Discard the water layer, add 1 mL of methanol, sonicate for 2 min, transfer the supernatant to a chromatographic bottle after magnetic separation, repea...

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Abstract

The invention provides a method for detecting phthalate in tobacco essence or water-based adhesive. The method comprises the following steps: weighing the tobacco essence or water-based adhesive, adding an organic solvent, carrying out oscillation extraction, taking a part of the extraction liquid and carrying out nitrogen blowing, carrying out water redissolution, carrying out magnetic graphene solid-phase extraction purification and elution, and determining phthalate in the tobacco essence or water-based adhesive by using gas chromatography-tandem mass spectrometry. The method can be used for rapidly and accurately detecting the residual amount of phthalate, and has the advantages of environmental protection, accurate result, less interference, high sensitivity and good repeatability. The method is especially suitable for detecting the residual phthalate in the tobacco essence or water-based adhesive.

Description

Technical field [0001] The present invention belongs to the technical field of physical and chemical inspection of hazardous substance residues in tobacco flavors or water-based gums, and mainly relates to a method for determining 13 kinds of phthalate esters in tobacco flavors or water-based gums, specifically after extraction with organic solvents , Purified by magnetic graphene solid phase extraction, and directly determined by gas chromatography-tandem mass spectrometry. Background technique [0002] Phthalates (PAEs) are a class of substances commonly referred to as plasticizers. They are used in industrial products to increase the transparency, durability, elasticity and longevity of plastic products, including personal care products, drugs, Food packaging, nutritional supplements, etc. However, studies have found that phthalates are biologically toxic. They can interfere with the normal regulation of the endocrine system, immunity and nerves, and have mutagenic, teratogen...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/7233G01N30/8637G01N2030/045G01N2030/062
Inventor 朱静陆冰琳许蔼飞杨飞宋凌勇农李政刘珊珊唐桂芳林莉潘玉灵
Owner CHINA TOBACCO GUANGXI IND