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GB 31604.13-2016 English PDF (GB31604.13-2016)

GB 31604.13-2016 English PDF (GB31604.13-2016)

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GB 31604.13-2016: Food contact materials -- Polymer -- Determination of 11-aminoundecanoic acid in food simulants -- High performance liquid chromatography

This standard specifies the test method of high performance liquid chromatography of 11-amino undecanoic acid migration quantity in food contact materials and products. This standard applies to the determination of 11-amino undecanoic acid migration quantity in food contact materials and products.
GB 31604.13-2016
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
National food safety standard -
Food contact materials and products - Determination
of 11-amino undecanoic acid migration quantity
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of the PRC
Table of Contents
Foreword . 3
1 Scope .. 4
2 Principles .. 4
3 Reagents and materials . 4
4 Instrument and equipment . 6
5 Analytical procedures . 7
6 Analysis results expression . 8
7 Precision . 9
8 Others . 9
Appendix A 11-amino undecanoic acid standard substance derivative
chromatogram . 10
Foreword
This standard replaces GB/T 23296.12-2009 "Food contact materials ?€? Polymer - Determination of 11-aminoundecanoic acid in food simulants - High
performance liquid chromatography"
Compared with GB/T 23296.12-2009, the main changes of this standard are as follows.
--- The standard name is changed to ?€?National food safety standard - Food contact materials and products - Determination of 11-amino undecanoic
acid migration quantity?€?;
--- Modify the preparation of food simulant test solution;
--- Modify the expression of analysis results.
National food safety standard -
Food contact materials and products - Determination
of 11-amino undecanoic acid migration quantity
1 Scope
This standard specifies the test method of high performance liquid
chromatography of 11-amino undecanoic acid migration quantity in food contact materials and products.
This standard applies to the determination of 11-amino undecanoic acid
migration quantity in food contact materials and products.
2 Principles
11-amino undecanoic acid in food simulants reacts with fluorescamine to form derivative, which is separated by high performance liquid chromatography; use fluorescence detector to test the derivative content; obtain the content of 11- amino undecanoic acid by conversion; use external standard method to quantify. 3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are analytical grade, the water is the grade-1 water specified in GB/T 6682. The containers and transfer apparatuses in the test shall avoid using plastic materials. 3.1 Reagents
3.1.1 Disodium tetraborate decahydrate (Na2B4O7??10H2O).
3.1.2 Phosphoric acid (H3PO4).
3.1.3 Boric acid (H3BO3).
3.1.4 Fluorescent amine (C17H10O4).
3.1.5 Sodium hydroxide (NaOH).
11-amino undecanoic acid (C11H23O2N, CAS No.. 2432-99-7), purity ??? 99%, or standard substance which is identified by national authentication and awarded a reference material certificate.
3.4 Standard solution preparation
3.4.1 11-amino undecanoic acid aqueous-solution stock solution (1.25mg/mL). Accurately WEIGH 125mg (accurate to 0.1mg) of 11-amino undecanoic acid
standards; USE 2mL of 96% acetic acid to dissolve it; TRANSFER it into 100mL volumetric flask; USE water to dilute it to the mark; STORE it in a refrigerator at 4 ??C.
3.4.2 11-amino undecanoic acid isooctane stock solution (0.50mg/mL).
Accurately WEIGH 25mg of 11-amino undecanoic acid standards (accurate to 0.1mg); USE 5mL of glacial acetic acid to dissolve it; TRANSFER it into 50mL volumetric flask; USE isooctane to dilute it to the mark; STORE it in a refrigerator at 4 ??C.
3.4.3 11-amino undecanoic acid aqueous-solution standard intermediate
solution (25??g/mL). Respectively MOVE 2mL of aqueous solution stock solution into 3 different 100mL volumetric flasks; USE water-based, acidic, alcoholic food simulants to dilute it, respectively.
3.4.4 Water-based, acidic food, alcoholic food simulants standard working solution. Respectively MOVE 0mL, 1.0mL, 2.0mL, 4.0mL, 10.0mL, 20.0mL of 11-amino undecanoic acid aqueous solution standard intermediate solution into 50mL volumetric flask; USE water to dilute it. The concentration of the standard working solution is 0??g/mL, 0.5??g/mL, 1.0??g/mL, 2.0??g/mL, 5.0??g/mL and
10.0??g/mL, respectively. In the same way, USE the corresponding acidic and alcoholic food simulants to prepare 11-amino undecanoic acid standard working solution with the same concentration series. PREPARE it when in use.
3.4.5 Oil-based food simulant standard working solution. WEIGH 5g (accurate to 0.01g) of olive oil respectively; PLACE it into 6 different 25mL conical flasks. Respectively ADD 0??L, 5??L, 10??L, 20??L, 50??L and 100??L of 11-amino
undecanoic acid isooctane stock solution; MIX it uniformly. The concentration of standard working solution is 0??g/g, 0.5??g/g, 1.0??g/g, 2.0??g/g, 5.0??g/g and 10.0??g/g, respectively. Then operate according to 5.2.2.
4 Instrument and equipment
4.1 High performance liquid chromatography. Equipped with fluorescence
detector.
4.2 Oscillator. Reciprocating-type.
Accurately MOVE 1.0mL of boric acid buffer solution into the prepared water- based, acidic, alcoholic, oil-based food simulant test solution and the prepared blank solution; PLACE it on vortex oscillator for 10s; MIX it uniformly. During the mixing process, ADD 1.0mL of fluorescamine solution. The resulting derivative solution is passed through microfiltration membrane; the filtrate is waiting for determination.
5.5 Instrument reference conditions
a) Chromatographic column. C18 column (column-length 250mm, inner-
diameter 4.6mm, particle-size 5??m), or the chromatographic column with
equivalent performance.
b) Mobile phase. methanol-phosphate buffer solution (70+30, volume ratio). c) Flow rate. 1.0mL/min.
d) Injection volume. 10??L.
e) Column temperature. room temperature.
f) Fluorescence detector. excitation wavelength 390nm, emission
wavelength 480nm.
5.6 Drawing of standard working curve
Respectively PIPETTE the above standard series of derivatization solution into liquid chromatograph; DETERMINE the corresponding peak area according to 5.5 instrument reference conditions (see Appendix A for the chromatogram of 11-amino undecanoic acid standard substance derivative). With the 11-amino undecanoic acid concentration of standard working solution as abscissa, AND the corresponding peak area of 11-amino undecanoic acid as vertical axis, DRAW a standard working curve.
5.7 Determination of sample solution
According to 5.5 instrument reference conditions, INJECT the sample derivative solution into liquid chromatograph; DETERMINE the nature based on the
retention time; at the same time, RECORD peak area; OBTAIN the
concentration of 11-amino undecanoic acid in the solution-under-test according to the standard curve.
6 Analysis results expression
OBTAIN 11-amino undecanoic acid concentration of food stimulant sample
solution from standard curve; CALCULATE migration quantity according to GB

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