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

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GB 5009.215-2016: Technical regulations for cotton processing
GB 5009.215-2016
NATIONAL STANDARD OF THE
PEOPLE’S 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’s 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 μm; 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 μL
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 μL 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 μL 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 μL 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 μm; 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; photomult...