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GB 5009.215-2016 English PDF (GB5009.215-2016)

GB 5009.215-2016 English PDF (GB5009.215-2016)

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GB 5009.215-2016: Technical regulations for cotton processing

This Standard specifies gas chromatography - pulse flame photometric detector detection method for organotin in food. This Standard is applicable to the determination of dimethyltin, trimethyltin, monobutyltin, dibutyltin, tributyltin, phenyltin, diphenyltin and triphenyltin in samples like fish, shellfish, wine and soy sauce.
GB 5009.215-2016
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
National Food Safety Standard -
Determination of Organotin in Food
ISSUED ON: AUGUST 31, 2016
IMPLEMENTED ON: MARCH 1, 2017
Issued by: National Health and Family Planning Commission of the
PEOPLE Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Instruments and Equipment ... 6
5 Analytical Procedures ... 7
6 Expression of Analytical Result ... 10
7 Precision ... 11
8 Others ... 11
Appendix A Preparation of Organotin Standard Solution ... 12
Appendix B Examples of Chromatogram ... 13
National Food Safety Standard -
Determination of Organotin in Food
1 Scope
This Standard specifies gas chromatography - pulse flame photometric detector detection method for organotin in food.
This Standard is applicable to the determination of dimethyltin, trimethyltin, monobutyltin, dibutyltin, tributyltin, phenyltin, diphenyltin and triphenyltin in samples like fish, shellfish, wine and soy sauce.
2 Principle
Respectively take monomethyltin as the internal standard of monosubstituted organotin; take tripropyltin as the internal standard of disubstituted organotin and trisubstituted organotin. Adopt internal standard method to quantify. In the sample, quantitatively add monomethyltin and tripropyltin internal standard. Through the assistance of ultrasound, extract organotin; use organic solvent to extract it. The extracted sample solution shall receive gel permeation chromatographic purification, pentyl Grignard reagent derivatization. The derivatized product shall receive Florisil purification. Adopt gas chromatography - pulse flame photometric detector (GC-PFPD) for determination.
3 Reagents and Materials
Unless it is otherwise stipulated, all reagents used in this Method shall be analytically pure. Water shall be Grade-1 water stipulated in GB/T 6682.
3.1 Reagents
3.1.1 N-hexane (n-C6H14): re-distilled.
3.1.2 Tetrahydrofuran (CH2CH2OCH2CH2): re-distilled.
3.1.3 Ethyl acetate (CH3COOC2H5): re-distilled.
3.1.4 Cyclohexane (C6H12): re-distilled.
3.1.5 Methanol (CH3OH).
3.1.6 Anhydrous ether (C2H5OC2H5).
3.3.1 Organotin standard substance and its standard solution: please refer to Appendix A. The purity of dimethyltin and tributyltin is 95%, other than this, the purity of other standard substances shall all be more than 97%.
3.3.2 Internal standard: monomethyltin (MMT) and tripropyltin (TPrT) standard substance: purity > 98%.
3.4 Preparation of Standard Solutions
3.4.1 Organotin standard stock solution: accurately weigh-take a proper amount of organotin standard substance, then, place it in a 10 mL beaker. Add methanol - aqueous solution (3.2.4) to dissolve it, then, transfer it to a 10 mL volumetric flask. In addition, dilute it to the scale. Store it in the refrigerator at -20 ??C. 3.4.2 Internal standard - standard stock solution: accurately weigh-take a proper amount of the internal standard, then, place it in a 10 mL beaker. Add methanol - aqueous solution (3.2.4) to dissolve it, then, transfer it to a 10 mL volumetric flask. In addition, dilute it to the scale. Store it in the refrigerator at -20 ??C. 3.4.3 Organotin standard and internal standard intermediate solution: measure-take a proper amount of organotin standard or internal standard stock solution. Use methanol - aqueous solution (3.2.4) to dilute it by 100 times. Please refer to Appendix for the mass concentration. Store it in the refrigerator at -20 ??C.
3.4.4 Organotin standard and internal standard working solution: measure-take a proper amount of organotin standard or internal standard intermediate solution; place it in a 10 mL volumetric flask. Add methanol - aqueous solution (3.2.4); dilute to the scale. Please refer to Appendix A for the concentration. Store it in the refrigerator at - 20 ??C.
4 Instruments and Equipment
4.1 Gas chromatograph (GC): equipped with pulse flame photometric detector (PFPD), sulfur filter.
4.2 Chromatographic column: DB-1 capillary column or equivalent column; column length: 30 m; membrane thickness: 0.25 ??m; internal diameter: 0.25 mm.
4.3 Tissue homogenizer.
4.4 Oscillator.
4.5 Ultrasonic cleaner.
4.6 Rotary evaporator.
4.7 Nitrogen concentrator.
and drying may be adopted to make freeze-dried powder. Place it at a low temperature of -20 ??C for storage.
5.2.1 Sample extraction
5.2.1.1 Fish sample
Accurately weigh-take a proper amount of sample; add 0.15 g of ethylene diamine tetra-acetic acid and 5 mL of 20 g/L sodium chloride solution; shake it up. Add 50 ??L of internal standard working solution; add 15 mL of hydrobromic acid - tetrahydrofuran solution (1 + 20) (3.2.5); conduct ultrasound for 5 min. If the sample is wet, add 1 mL of saturated sodium chloride solution; shake it up. Then, add 50 ??L of internal standard working solution; add 15 mL of hydrobromic acid - tetrahydrofuran solution (1 + 20) (3.2.5); conduct ultrasound for 5 min.
5.2.1.2 Shellfish sample
Accurately weigh-take a proper amount of sample; add 5 mL of 20% sodium chloride solution; shake it up. Add 50 ??L of internal standard working solution; add 15 mL of hydrobromic acid - tetrahydrofuran solution (1 + 20) (3.2.5); conduct ultrasound for 5 min.
5.2.1.3 Liquid sample, for example, wine
Measure-take 10 mL of sample; add 2 g of sodium chloride; shake it up. Add 50 ??L of internal standard working solution; add 15 mL of hydrobromic acid - tetrahydrofuran solution (1 + 20) (3.2.5); conduct ultrasound for 5 min.
5.2.2 Purification of sample solution
Add 25 mL of n-hexane, which contains 0.03% tropolone, to the sample solution. Conduct oscillating extraction for 40 min; conduct centrifugation for 10 min (at 3,000 r/min). Place it still for stratification. Absorb organic phase, then, transfer it to an eggplant-shaped bottle. Add 10 mL of n-hexane to the residue; conduct oscillating extraction for 10 min. Conduct centrifugation for 10 min (at 3,000 r/min); place it still for stratification; extract the organic phase. Combine them in the eggplant-shaped bottle; conduct rotary evaporation and concentration, till it reaches near dryness. 5.2.3 Gel permeation chromatographic purification
5.2.3.1 Filling of gel column: take polystyrene gel; use tetrahydrofuran - ethyl acetate (1 + 1) solution to soak it overnight. Use glass wool to block the bottom of the glass chromatographic column whose internal diameter is 1.7 cm ~ 1.8 cm. Through wet process, add the previously soaked gel. The gel naturally settles. After it becomes stabilized, the column length is around 15 cm.
5.2.3.2 Purification: add 1 mL of tetrahydrofuran - ethyl acetate (1 + 1) solution to the a) Chromatographic column1: DB-1 column (or equivalent column); column length: 30 m; membrane thickness: 0.25 ??m; internal diameter: 0.25 mm.
b) Adopt the mode of no-splitting; sample inlet temperature: 280 ??C.
c) Colum temperature program: initial temperature: 50 ??C, maintain for 1 min; at 10 ??C/min, raise the temperature to 120 ??C; at 5 ??C/min, raise the temperature to 200 ??C; at 10 ??C/min, raise the temperature to 280 ??C; maintain for 5 min. d) Carrier gas is high-purity nitrogen (purity > 99.999%).
e) Pulse flame photometric detector reference conditions: pattern: sulfur filter; temperature: 350 ??C; flow rate of fuel gas and oxidant gas: air1 21 mL/min, hydrogen 22 mL/min, air2 11 mL/min; photomultiplier voltage: 550 V; threshold time: 4 ms; gate delay time: 5 ms; excitation voltage: 100 mV.
5.4 Draw a Standard Curve
Accurately weigh-take corresponding food sample, which does not contain organotin, as a proper amount of blank matrix. Add 5 mL of 20% sodium chloride solution; respectively add 0 ??L, 10 ??L, 30 ??L, 50 ??L, 100 ??L, 200 ??L and 400 ??L of organotin mixed standard solution, and 50 ??L of internal standard working solution. In accordance with the requirements of the sample extraction and purification process, operate synchronously. Absorb 1 ??L of the standard series solution; inject it into the gas chromatograph for analysis. Thus, obtain its chromatogram (please refer to Appendix B.1 and Appendix B.2); use the retention time for qualitative determination. 5.5 Determination of Sample Solution
Absorb 1 ??L of the sample solution, then, inject it into the gas chromatograph. Thus, obtain its chromatogram (please refer to Appendix B.3); use the retention time for qualitative determination. Calculate the peak area ratio or peak height ratio of target chemical compound and internal standard. Use the peak area ratio or peak height ratio of the sample injection volume (ng) of target organotin in the standard series solution and corresponding target organotin and internal standard to draw a linear curve. In accordance with the linear curve, calculate the content of organotin in the sample. 6 Expression of Analytical Result
The mass fraction of target organotin (counted by Sn) in the sample shall be calculated in accordance with Formula (1):
1 This information is provided to make it convenient for the users of this Standard. It does not signify approval of the product. If other equivalent products have the same effect, then, these equivalent products may also be adopted.

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