Method for measuring bisphenol A in product by gas chromatography-mass spectrometry

A gas chromatography and mass spectrometry technology, applied in the detection field of bisphenol A in products, can solve the problems of high solvent consumption, unsatisfactory detection effect and high detection cost in liquid chromatography analysis, and achieves low detection limit and low interference. , The effect of low detection cost

Inactive Publication Date: 2010-05-05
NINGBO PTS PROD TECH SERVICE
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

EU 2002 / 72 / EC regulations stipulate that the migration limit of bisphenol A in plastic food contact materials is 3mg / kg; Canada banned bisphenol A in containers such as feeding bottles and water bottles in February 2009; in May 2009 and In June, Minnesota and Connecticut also banned the use of bisphenol A in certain products, becoming the first two states in the United States to ban bisphenol A. Therefore, the detection of bisphenol A in products has become an international research topic. It is a hot topic, but there are still few research reports on the detection of bisphenol A in my country. The European Union uses liquid chromatography to detect the migration of bisphenol A, but the detection limit is only 0.2-0.7 mg / kg, and the detection effect is not very ideal. , and the use of liquid chromatographic analysis requires a large amount of solvent consumption and high detection costs

Method used

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  • Method for measuring bisphenol A in product by gas chromatography-mass spectrometry
  • Method for measuring bisphenol A in product by gas chromatography-mass spectrometry
  • Method for measuring bisphenol A in product by gas chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Accurately weigh 1.0mg of bisphenol A, dissolve it with an appropriate amount of acetone, transfer it to a 200ml volumetric flask, and dilute to the mark with acetone. Shake well and let stand to get 5μg / ml BPA standard solution. The solution used for the test working curve of BPA is diluted step by step from the above 5μg / ml standard solution, respectively prepared into a series of solutions of 0.1, 0.2, 0.5, 1.0, 2.0μg / ml, and hexamethyldisilazane is added to bisphenol A Carry out silanization derivation, the derivative liquid is filtered through a 0.45 μm needle-type organic phase filter head, and then analyzed and detected by gas chromatography-mass spectrometry instrument GC-MS according to the above experimental conditions, wherein the gas chromatography-mass spectrometry instrument inlet temperature is set to The temperature at the interface of the gas chromatograph-mass spectrometer is set at 280°C; the carrier gas is high-purity helium, and the flow rate is 1 m...

Embodiment 2

[0026] Measure a polycarbonate sample of 100 square centimeters in a 500ml beaker, add a corresponding amount of acetone in the ratio of area:solvent=1:2 (square centimeter:milliliter), soak and extract at 40°C for 4 hours (the sample needs to be completely immersion). After filtering the extract, take 5ml into a 20ml headspace bottle, add 400μl of hexamethyldisilazane, and derivatize at 50°C for 5 hours. After the derivative liquid is filtered through a 0.45 μm needle-type organic phase filter head, the filtered extract is tested and analyzed by a gas chromatography-mass spectrometer, and the test and analysis experimental conditions of the gas chromatography-mass spectrometer are the same as in Example 1. Quantification by external standard method. Three parallel samples were made to the polycarbonate sample, the test numbers were A, B, and C, and the analysis results were shown in Table 1, and the first parallel sample (test number A) was measured 5 times, and the analysis...

Embodiment 3

[0032] The standard solution in Example 1 was added to the prepared test solution with known negative results (the test did not contain the target compound), and the experiment was carried out according to the instrumental analysis and detection method in Example 1. This sample is done 10 parallel measurements to get the average value, according to the actual addition amount and the measured results, calculate the standard recovery rate of this sample, the test results are shown in Table 3, as can be seen from Table 3, the standard recovery rate of the sample reaches 87-94%. %, the relative standard deviation of parallel measurements was 2.2%.

[0033]Table 3 The recovery of standard addition of this sample

[0034] serial number

[0035] serial number

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Abstract

The invention discloses a method for measuring bisphenol A in a product by gas chromatography-mass spectrometry. The method comprises the following steps of: soaking and extracting bisphenol A in a sample with an organic solvent, and then carrying out silanization and derivatization; detecting the bisphenol A in the sample with a gas chromatography-mass spectrometer: setting the temperature of a sample injection port to be 250-300 DEG C, a flow rate to be 0.8-1.5ml / min and the temperature of a port to be 280-300 DEG C; enabling the sample to enter the sample injection port, carrying out temperature programming on the temperature of the chromatographic column from 40-60 DEG C to 250-320 DEG C; and enabling the sample to enter a mass spectrometric detection part through the port to carry out mass spectrometric detection, wherein an electron impact ion source is adopted as the ion source of the mass spectrometric detection, the impact energy of the ion source is 70eV, and the temperature of the ion source is set to be 230-250 DEG C. The method for measuring the bisphenol A in the product has low detection limit, good detection effect, little consumption of analysis solvent and low detection cost.

Description

technical field [0001] The invention relates to a method for detecting bisphenol A in products, in particular to a method for detecting bisphenol A in products by gas chromatography-mass spectrometry. Background technique [0002] Bisphenol A (Bisphenol A, referred to as BPA) scientific name 2,2-bis (4-hydroxyphenyl) propane, referred to as bisphenol propane, is an important organic chemical raw material, an important derivative of phenol and acetone, mainly used in the production of Polycarbonate, epoxy resin, polysulfone resin, polyphenylene ether resin, unsaturated polyester resin and other polymer materials. It can also be used in the production of plasticizers, flame retardants, antioxidants, heat stabilizers, rubber antioxidants, pesticides, coatings and other fine chemical products. [0003] Many independent institutions or toxicology experts have clearly stated that bisphenol A is harmful to the human body, especially to children. Their research shows that bisphenol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/54G01N30/28
Inventor 刘展李向红陆斌李伟朱利平盛李建
Owner NINGBO PTS PROD TECH SERVICE
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