A method for simultaneous determination of three kinds of bisphenols content

Abstract

The invention discloses a method for simultaneously measuring the content of three bisphenol substances, which comprises the steps of filtering a sample solution by an aqueous microporous membrane, adding an extractant and an emulsifier, eddying to form a uniform emulsion, adding hydrochloric acid for centrifugal phase splitting after standing, and taking an upper extracted phase to measure the content of bisphenol A, bisphenol AF and tetrabromobisphenol A by adopting high performance liquid chromatography. According to the invention, the extractant is binary or ternary mixture of n-caprylic acid, nonanoic acid, capric acid, undecanoic acid and lauric acid. The emulsifier is ammonium hydroxide or sodium hydroxide. The mixture of various aliphatic acids is taken to prepare an eutectic solvent serving as the extractant, alkali is taken as the emulsifier for the first time, the extracted object is fully contacted with the extractant, the extraction is completely carried out, and the content of the three low-content bisphenol substances in food and food packaging materials can be accurately detected simultaneously. The method has the characteristics of fast and uniform emulsion formation, quick and complete phase splitting, high efficiency, low toxicity, simple operation, high sensitivity, good reproducibility and the like.

Description

technical field

[0001] The invention belongs to the technical field of harmful substance residue detection, and in particular relates to a method capable of simultaneously and accurately detecting the content of three kinds of bisphenols in food or food packaging materials. Background technique

[0002] Bisphenol A (BPA) is a raw material for polycarbonate plastics and epoxy coatings, and is widely used in food contact materials. Studies have shown that bisphenol A has a certain endocrine disrupting effect, especially on infants and young children. Therefore, the European Union, Japan, China, and the United States have strictly restricted the use of bisphenol A in food contact materials. At present, manufacturers often replace bisphenol A with bisphenol AF (BPF) or tetrabromobisphenol A, which is similar in structure and performance to bisphenol A. However, studies have shown that bisphenol AF and tetrabromobisphenol A also have a certain degree of human health hazards. Th...

Examples

Embodiment 1

[0016] Example 1: Detection of bisphenol A content in bottled water and buckets

[0017] 1. Preparation of deep eutectic solvent: Mix n-octanoic acid and n-decanoic acid in a molar ratio of 2:1, heat to 70°C to form a uniform transparent solution, that is, form a deep eutectic solvent.

[0018] 2. Working curve making: prepare 0.1, 0.5, 1, 2, 5, 10, 20 μg / mL bisphenol A standard solutions respectively, liquid chromatography conditions: mobile phase is acetonitrile-water, V (acetonitrile): V (water )=60:40, flow rate 1mL / min, detection wavelength 224nm, autosampler injection, injection volume 10μL. Its linear range, regression equation and correlation coefficient are shown in Table 1.

[0019] Table 1 Bisphenols linear range, regression equation, correlation coefficient

[0020]

[0021] Table 2 bisphenols standard addition recovery (%) n=6

[0022]

[0023]

[0024] 3. Determination of bisphenol A in bottled water: Take 50mL bottled water, filter it through a 0.45μ...

Embodiment 2

[0026] Embodiment 2: the mensuration of bisphenol A and bisphenol AF content in canned pork

[0027] 1. Preparation of deep eutectic solvent: Mix n-nonanoic acid, n-decanoic acid, and undecanoic acid in a molar ratio of 3:1:1, heat to 75°C to form a uniform transparent solution, that is, form a deep eutectic solvent.

[0028] 2. Preparation of working curves: Prepare 0.1, 0.5, 1, 2, 5, 10, 20 μg / mL bisphenol A and bisphenol AF mixed standard solutions respectively. See Table 1 for the linear range, regression equation and correlation coefficient. Rates are shown in Table 2. Chromatographic conditions: AgilentEclipse plus C18 column (2.1mm×100mm, 3.5μm), column temperature is 30°C; mobile phase A is water, mobile phase B is methanol, gradient elution; gradient elution program is: (0-3 ) min, 50% B, (3-7) min, 50% B-80% B, (7-15) min, 80% B, (3-7) min, 80% B-50% B; the flow rate is 1.0mL / min; detection wavelength: 280nm; injection volume: 10μL.

[0029] 3. Pretreatment of can...

Embodiment 3

[0033] Embodiment 3: Determination of bisphenols in plastic packaging materials

[0034] 1. Preparation of deep eutectic solvent: Mix n-nonanoic acid, undecanoic acid, and dodecanoic acid in a molar ratio of 2:1:1, and heat to 80°C to form a uniform transparent solution, that is, a deep eutectic solvent.

[0035] 2. Working curve creation: prepare 0.1, 0.5, 1, 2, 5, 10, 20 μg / mL bisphenol A, bisphenol AF, tetrabromobisphenol A mixed standard solutions respectively, see the linear range, regression equation and correlation coefficient Table 1, the recovery rate of standard addition is shown in Table 2, and the chromatograms of 0.50 μg / kg bisphenol A, bisphenol AF and tetrabromobisphenol A treated with micro-extraction of the present invention and without micro-extraction are shown in Table 2. figure 1 , the chromatographic conditions are the same as in Example 2.

[0036] 3. Pretreatment of samples of bisphenols in plastic packaging materials: crush the samples of plastic pack...

technical field

[0001] The invention belongs to the technical field of harmful substance residue detection, and in particular relates to a method capable of simultaneously and accurately detecting the content of three kinds of bisphenols in food or food packaging materials. Background technique

[0002] Bisphenol A (BPA) is a raw material for polycarbonate plastics and epoxy coatings, and is widely used in food contact materials. Studies have shown that bisphenol A has a certain endocrine disrupting effect, especially on infants and young children. Therefore, the European Union, Japan, China, and the United States have strictly restricted the use of bisphenol A in food contact materials. At present, manufacturers often replace bisphenol A with bisphenol AF (BPF) or tetrabromobisphenol A, which is similar in structure and performance to bisphenol A. However, studies have shown that bisphenol AF and tetrabromobisphenol A also have a certain degree of human health hazards. Th...

Examples

Embodiment 1

[0016] Example 1: Detection of bisphenol A content in bottled water and buckets

[0017] 1. Preparation of deep eutectic solvent: Mix n-octanoic acid and n-decanoic acid in a molar ratio of 2:1, heat to 70°C to form a uniform transparent solution, that is, form a deep eutectic solvent.

[0018] 2. Working curve making: prepare 0.1, 0.5, 1, 2, 5, 10, 20 μg / mL bisphenol A standard solutions respectively, liquid chromatography conditions: mobile phase is acetonitrile-water, V (acetonitrile): V (water )=60:40, flow rate 1mL / min, detection wavelength 224nm, autosampler injection, injection volume 10μL. Its linear range, regression equation and correlation coefficient are shown in Table 1.

[0019] Table 1 Bisphenols linear range, regression equation, correlation coefficient

[0020]

[0021] Table 2 bisphenols standard addition recovery (%) n=6

[0022]

[0023]

[0024] 3. Determination of bisphenol A in bottled water: Take 50mL bottled water, filter it through a 0.45μ...

Embodiment 2

[0026] Embodiment 2: the mensuration of bisphenol A and bisphenol AF content in canned pork

[0027] 1. Preparation of deep eutectic solvent: Mix n-nonanoic acid, n-decanoic acid, and undecanoic acid in a molar ratio of 3:1:1, heat to 75°C to form a uniform transparent solution, that is, form a deep eutectic solvent.

[0028] 2. Preparation of working curves: Prepare 0.1, 0.5, 1, 2, 5, 10, 20 μg / mL bisphenol A and bisphenol AF mixed standard solutions respectively. See Table 1 for the linear range, regression equation and correlation coefficient. Rates are shown in Table 2. Chromatographic conditions: AgilentEclipse plus C18 column (2.1mm×100mm, 3.5μm), column temperature is 30°C; mobile phase A is water, mobile phase B is methanol, gradient elution; gradient elution program is: (0-3 ) min, 50% B, (3-7) min, 50% B-80% B, (7-15) min, 80% B, (3-7) min, 80% B-50% B; the flow rate is 1.0mL / min; detection wavelength: 280nm; injection volume: 10μL.

[0029] 3. Pretreatment of can...

Embodiment 3

[0033] Embodiment 3: Determination of bisphenols in plastic packaging materials

[0034] 1. Preparation of deep eutectic solvent: Mix n-nonanoic acid, undecanoic acid, and dodecanoic acid in a molar ratio of 2:1:1, and heat to 80°C to form a uniform transparent solution, that is, a deep eutectic solvent.

[0035] 2. Working curve creation: prepare 0.1, 0.5, 1, 2, 5, 10, 20 μg / mL bisphenol A, bisphenol AF, tetrabromobisphenol A mixed standard solutions respectively, see the linear range, regression equation and correlation coefficient Table 1, the recovery rate of standard addition is shown in Table 2, and the chromatograms of 0.50 μg / kg bisphenol A, bisphenol AF and tetrabromobisphenol A treated with micro-extraction of the present invention and without micro-extraction are shown in Table 2. figure 1 , the chromatographic conditions are the same as in Example 2.

[0036] 3. Pretreatment of samples of bisphenols in plastic packaging materials: crush the samples of plastic pack...

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