BHA detection of food additive tert-butyl-4-hydroxyanisole

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A. 1 General regulations

When no other requirements are specified, the reagents and water used in this standard refer to analytical pure reagents and Grade III water specified in GB/T6682. The standard titration solution, impurity determination standard solution, formulation, and product used in the experiment shall be prepared in accordance with the provisions of GB/T601, GB/T602, and GB/T603 unless other requirements are specified. The solution used in the experiment refers to aqueous solution when no specific solvent is specified for preparation

A.2 Identification Test

A.2.1 Solubility

Insoluble in water, easily soluble in ethanol and propylene glycol.

A.2.2 Color Reaction

A.2.2.1 Reagents and Materials

A.2.2.1.1; Ethanol solution: 72% (volume fraction)

A.2.2.1.2; 2,6-Dichloroquinone chloroimine solution: Weigh 0.1g; Dissolve 2,6-dichloroquinone chloroimine in 1000mL of anhydrous ethanol

A.2.2.1.3 Sodium borate solution: Weigh 2g of sodium borate (Na2Ba4O7 · 10H2O) and dissolve it in 100mL of water

A.2.2.2 Identification

Weigh 0.1g of the sample, dissolve it in 1000mL of ethanol solution, take 5mL of this solution, add 2mL of sodium borate solution and 1mL; 2,6-Dichloroquinone chloroimine solution, mixed, should appear blue

A.3; Determination of Butylhydroxyanisole (C11H16O2) Content

A.3.1 Reagents and Materials

A.3.1.1  4-tert butylphenol

A.3.1.2; Acetone

A.3.1.3 Standards for 3-tert-butyl-4-hydroxyanisole (3-BHA) and 2-tert-butyl-4-hydroxyanisole (2-BHA)

A.3.2 Instruments and Equipment

Gas chromatograph: equipped with a hydrogen flame ionization detector.

A.3.3 Reference chromatographic conditions

A.3.3.1 Column: 1.8m × 2mm (inner diameter) stainless steel column or other equivalent chromatographic column, filled with 10% GE XE-60 silicone resin or other equivalent

A.3.3.2 Flow rate: 30mL/min

A.3.3.3 Column temperature: 175 ℃~185 ℃

A.3.3.4 Carrier gas: Helium

A.3.3.5 Injection volume: 5uL

Analysis steps in A.3.4

Preparation of internal standard solution in A.3.4.1

Weigh approximately 500mg of 4-tert butylphenol (accurate to 0.2mg), dissolve in acetone, and dilute to 100mL

A.3.4.2 Preparation of Standard Solution

Weigh approximately 90mg of 3-tert butyl-4-hydroxyanisole (3-BHA) standard and approximately 10mg of 2-tert butyl-4-hydroxyanisole (2-BHA) standard (accurate to 0.2mg), dissolve with internal standard solution and bring to volume to 10mL, so that the final concentrations of 3-BHA and 2-BHA are 9mg/mL and 1mg/mL, respectively

A.3.4.3 Preparation of Sample Solution

Weigh approximately 100mg of the sample (accurate to 0.2mg), dissolve it with an internal standard solution, and dilute to 10mL.

A.3.4.4 Determination

Under the reference chromatographic conditions of A.3.3, inject about 5uL of standard solution and sample solution respectively, and record the chromatogram.

. Measure the peak area of each isomer

A.3.5 Result Calculation

The mass fraction wi of each isomer in the sample is calculated according to equation (A.1):

Where:

pi - the mass concentration of 3-BHA or 2-BHA in the standard solution, in milligrams per milliliter (mg/mL)

Ru - the ratio of the peak area of 3-BHA or 2-BHA in the chromatogram of the sample solution to the peak area of the internal standard solution

R - The ratio of the peak area of 3-BHA or 2-BHA in the standard solution chromatogram to the peak area of the internal standard solution

10- The volume of the sample at constant volume after treatment, in milliliters (mL)

m1- The mass of the sample, in milligrams (mg)

The sum of the contents of the two isomers 3-BHA and 2-BHA calculated from equation (A.1) is the content of butyl hydroxyanisole (C11H16O2)

A.4 Determination of sulfuric acid ash

A.4.1 Reagents and materials

Concentrated sulfuric acid

A.4.2 Instruments and Equipment

A.4.2.1 Crucible: Quartz or platinum crucible.

A.4.2.2 Desiccator (using discolored silicone as desiccant)

A.4.2.3 High temperature furnace

A.4.3 Analysis Steps

Weigh approximately 5g of the sample to the nearest 0.0001g, place it in a constant weight crucible, and slowly ignite until complete carbonization occurs.

. Let it cool, add 0.5mL~1.0mL of concentrated sulfuric acid to moisten it, heat it at low temperature until all smoke is removed, and then burn it in an 800 ℃± 25 ℃ high-temperature furnace until it is completely ashed. Take it out, cool it in a dryer, and weigh it. Then burn at 800 ℃± 25 ℃ for constant weight

A.4.4 Result Calculation

The mass fraction w of sulfuric acid ash is calculated according to equation (A.2):

In the equation:

m3- the mass of the sample and crucible after ignition, in grams (g)

m2- Mass of the crucible, in grams (g)

m4- The mass of the sample and crucible before ignition, in grams (g)

The experimental results shall be based on the arithmetic mean of the results of two parallel measurements (to two decimal places). The absolute difference between two independent measurement results obtained under repeatability conditions shall not exceed 10% of the arithmetic mean

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