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Method for analyzing five colopholic acids in product by virtue of high performance liquid chromatography-tandem mass spectrometry

A high-performance liquid chromatography and tandem mass spectrometry technology, applied in the fields of analysis of materials, material separation, instruments, etc., can solve the problems of inability to detect and separate rosin acid, insufficient detection coverage, etc., and achieve low cost, low detection limit, and high precision. Effect

Active Publication Date: 2017-06-13
COMPREHENSIVE TECH SERVICE CENT OF QUANZHOU ENTRY EXIT INSPECTION & QUARANTINE BUREAU OF P R C
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are two deficiencies in these methods: first, the detection method only involves abietic acid and dehydroabietic acid in abietic acid, and abietic acid contains many substances, and the detection coverage is insufficient; second, abietic acid widely exists in various In a variety of daily consumer products, such as adhesives in shoe materials, paper, rosin soap, ink, etc.
This method cannot detect and separate the five kinds of abietic acids, which has certain limitations

Method used

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  • Method for analyzing five colopholic acids in product by virtue of high performance liquid chromatography-tandem mass spectrometry
  • Method for analyzing five colopholic acids in product by virtue of high performance liquid chromatography-tandem mass spectrometry
  • Method for analyzing five colopholic acids in product by virtue of high performance liquid chromatography-tandem mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] The detection of abietic acid in embodiment 1 adhesive

[0086] Accurately weigh 1g of the 309 adhesive sample, place it in a tubular hard glass extractor, add 10mL tert-butyl methyl ether, conduct the first ultrasonic extraction at 60°C for 30min, and filter; add 3mL tert-butyl methyl ether to the sample again, Carry out ultrasonic extraction for the second time at 60°C for 30 min, and filter; the filtrates from the two filtrations are combined and concentrated, and a mixed solvent of acetonitrile-0.3% acetic acid aqueous solution (V / V=65 / 35) is added in a 25mL volumetric flask to determine After the sample solution was filtered through a 0.45 μm organic filter membrane, it was measured by HPLC-MS, and the specific ion pair of the two-stage mass spectrum was selected, qualitatively according to the retention time of the chromatographic peak, and quantified by the peak area external standard method;

[0087] Liquid chromatography conditions:

[0088] Liquid chromatograph...

Embodiment 2

[0107] The detection of abietic acid in embodiment 2 paper

[0108] Cut the paper into small pieces of about 1mm×1mm, accurately weigh 1g of the paper sample, place it in a tubular hard glass extractor, add 10mL of methanol-water mixed solvent (V / V=75 / 25), and Carry out ultrasonic extraction for the first time at 60°C for 30min, filter; add 10mL methanol-water mixed solvent (V / V=75 / 25) to the sample again, carry out ultrasonic extraction for the second time at 60°C for 30min, filter; The filtrates of the first filtration were combined and then concentrated, added a mixed solvent of acetonitrile-0.3% acetic acid aqueous solution (V / V=65 / 35) to dissolve, then constant volume was carried out in a 25mL volumetric flask, and the sample solution was filtered through a 0.45 μm organic filter membrane , use HPLC-MS to measure, select the specific ion pair of the two-stage mass spectrum, qualitative according to the retention time of the chromatographic peak, and quantify with the exte...

Embodiment 3

[0126] The detection of abietic acid in embodiment 3 rosin soap

[0127] Cut the rosin soap into small fragments of about 1mm×1mm, accurately weigh 1g of the sample, place it in a tubular hard glass extractor, add 10mL of acetonitrile-0.3% acetic acid aqueous solution (V / V=65 / 35), and Carry out ultrasonic extraction for the first time at 60°C for 30 minutes, filter; add 10 mL of acetonitrile-0.3% acetic acid aqueous solution (V / V=65 / 35) to the sample again, carry out ultrasonic extraction for the second time at 60°C for 30 minutes, and filter; After the filtrates of the second filtration are combined, add a mixed solvent of acetonitrile-0.3% acetic acid aqueous solution (V / V=65 / 35) and carry out constant volume to 25mL in a volumetric flask. MS is used for determination, and specific ion pairs of two-stage mass spectrometry are selected, qualitatively according to the retention time of chromatographic peaks, and quantified by external standard method of peak area;

[0128] Li...

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Abstract

The invention provides a method for analyzing five colopholic acids in a product by virtue of a high performance liquid chromatography-tandem mass spectrometry, relating to a detection and analysis method for four products including adhesives, paper, rosin soap and printing ink as well as five colopholic acids including abietic acid, neoabietic acid, levopimaric acid, pimaric acid and dehydroabietic acid for shoe materials. The method comprises the steps of after a sample is preprocessed, adding an extraction solvent, carrying out ultrasonic extraction, filtering to obtain an extraction solution, concentrating the extraction solution to a definite volume, and carrying out detection and analysis by virtue of the high performance liquid chromatography-tandem mass spectrometry. The method provided by the invention is simple and convenient, the steps are few, a test result is accurate, and the detection effects of the five colopholic acids are good.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to a high-performance liquid chromatography tandem mass spectrometry analysis method for five kinds of abietic acids in a product. Background technique [0002] Rosin has excellent properties such as adhesion, anticorrosion, and insulation, and is widely used in the fields of adhesives, plastics, coatings, inks, papermaking, and medicine. In everyday consumer products, rosin may be found in products such as soap, paper, paint, and various shoes and toys that use adhesives and plastics. While rosin is widely used, its harmfulness has gradually been discovered and paid attention to by people. Rosin steam can cause acute poisoning symptoms such as headache, dizziness, cough, and asthma. It has been reported that the toxicity of resin acid to fish is 0.44μg / mL. Toxicological studies have shown that abietic acid can cause the dissolution of human alveolar ep...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/14G01N30/72
CPCG01N30/02G01N30/14G01N30/72G01N2030/062
Inventor 毛树禄绉强连小彬荣杰峰黄秋兰陈斌
Owner COMPREHENSIVE TECH SERVICE CENT OF QUANZHOU ENTRY EXIT INSPECTION & QUARANTINE BUREAU OF P R C
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