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Method for detecting bisphenol A

A bisphenol and sample technology, applied in the field of detection of bisphenol A, can solve the problems of low accuracy and sensitivity of titration method, inability to use trace samples for detection, long pretreatment time, etc., and achieve simple sample pretreatment and lower detection limit. , the effect of high sensitivity

Inactive Publication Date: 2019-03-29
HARBIN MEDICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the titration method is used for the detection of PC material baby bottles in my country. The pretreatment of samples requires multiple extractions and multiple centrifugations. The operation is cumbersome, the pretreatment time is long, the accuracy and sensitivity of titration are low, and it cannot be used for trace samples. detection

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  • Method for detecting bisphenol A
  • Method for detecting bisphenol A
  • Method for detecting bisphenol A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 standard curve drawing and sensitivity detection

[0033] Accurately weigh the appropriate amount of BPA, and prepare reference solution with concentrations of 56 μg / mL, 28 μg / mL, 14 μg / mL, 7 μg / mL, 3.5 μg / mL and 1.75 μg / mL. Into the aqueous hydrochloric acid solution with pH 1-2, slowly add 5 mL of 0.5 mmol aniline solution dropwise, and mix well. Stir in an ice bath, then add 5mL of 0.5mmol sodium nitrite solution dropwise, after fully reacting for 30min, adjust the pH value of the solution to 8-10 with sodium hydroxide, slowly add 5mL of the above-mentioned bisphenol A reference solution of different concentrations dropwise , concentrated to dryness after reacting for 20 minutes to obtain a derivatized product, after constant volume with chromatographic methanol, filtered through a 0.45 μm organic membrane, discarded the initial filtrate, and then analyzed the sample solution using high-performance liquid chromatography-ultraviolet / fluorescence detection me...

Embodiment 2

[0044] Prepare 4-6mmol hydrochloric acid into a hydrochloric acid solution with a pH of 1-2, slowly add 0.5mmol aniline solution dropwise, and mix well. Under stirring in an ice bath, 0.5 mmol of sodium nitrite solution was added dropwise. After fully reacting for 30 minutes, the pH value of the solution was adjusted to 9 with sodium hydroxide, and 100 mL of drinking water was slowly added dropwise. After reacting for 20 minutes, it was concentrated to dryness to obtain a derivatized product. After constant volume with chromatographic methanol, filter with 0.45 μm organic membrane, discard the primary filtrate, and use high performance liquid chromatography-ultraviolet / fluorescence detection method to analyze the sample solution in the subsequent filtrate, and calculate the content of bisphenol A in the sample. The results are shown in Table 1.

[0045] The chromatographic column is a C18 liquid chromatographic column, the flow rate is 1.0mL / min, the injection volume is 10μL, ...

Embodiment 3

[0047] Prepare 4-6mmol hydrochloric acid into a hydrochloric acid solution with a pH of 1-2, slowly add 0.5mmol aniline solution dropwise, and mix well. Under stirring in an ice bath, 0.5 mmol of sodium nitrite solution was added dropwise. After fully reacting for 30 minutes, the pH value of the solution was adjusted to 9 with sodium hydroxide, and 100 mL of distilled water was slowly added dropwise. After reacting for 20 minutes, it was concentrated to dryness to obtain a derivatized product. After constant volume of chromatographic methanol, filter with 0.45 μm organic membrane, discard the primary filtrate, and analyze the sample solution with high performance liquid chromatography-ultraviolet / fluorescence detection method in the subsequent filtrate, and calculate the content of bisphenol A in the sample. The results are shown in Table 1. The HPLC chromatogram of the derivative product of BPA in aniline and distilled water is as follows: figure 2 shown.

[0048] The chro...

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Abstract

The invention discloses a method for detecting bisphenol A (BPA). The method employs pre-column derivative-high performance liquid chromatography (HPLC) for detection. The method comprises the following steps of: using an aniline compound as a derivatization reagent to react with bisphenol A to generate a diazo compound; and analyzing derivatized product by HPLC to obtain the BPA content in a sample. The principle is that the BPA has stronger ultraviolet or fluorescence absorption after reacting with the derivatization reagent to generate the diazo compound, so as to reduce the detection limitand improve the sensitivity. The method has the advantages of low detection limit, high sensitivity, and simple operation, and capable of accurately quantitatively detecting the BPA in the sample. The detection limit of the method is 0.18ng, and the quantitative limit is 0.54ng. The detection limit is lower compared to the HPLC direct assay. The method disclosed by the invention can be used in the field of food safety detection, such as a food packaging material and a limit check of BPA in food.

Description

technical field [0001] The invention relates to a method for detecting bisphenol A, in particular to a method for detecting bisphenol A by pre-column derivatization-HPLC, which can be used for the limited inspection of bisphenol A in the field of food safety. Background technique [0002] Food safety is one of the most concerned issues in today's society, and the hygiene and safety of food packaging materials is an important aspect of food safety. The scientific name of bisphenol A is 2,2-bis(4-hydroxyphenyl)propane, referred to as diphenol Propane, also known as BPA, is an exogenous endocrine disruptor, an additive to synthetic plastic packaging products, which can migrate into food or beverages through food packaging and plastic films, be absorbed by the human body, and gradually harm human health. The harm of BPA has attracted widespread attention of the World Health Organization, and many countries have promulgated relevant laws to prohibit the addition of BPA-containin...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/067
Inventor 王立波李洋洋王金辉杨异卉甘春丽黄健蔺聪聪
Owner HARBIN MEDICAL UNIVERSITY
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