1
/
von
9
PayPal, credit cards. Download editable-PDF and invoice in 1 second!
GB 5009.189-2023 English PDF (GB5009.189-2023)
GB 5009.189-2023 English PDF (GB5009.189-2023)
Normaler Preis
$230.00 USD
Normaler Preis
Verkaufspreis
$230.00 USD
Grundpreis
/
pro
Versand wird beim Checkout berechnet
Verfügbarkeit für Abholungen konnte nicht geladen werden
Delivery: 3 seconds. Download true-PDF + Invoice.
Get QUOTATION in 1-minute: Click GB 5009.189-2023
Historical versions: GB 5009.189-2023
Preview True-PDF (Reload/Scroll if blank)
GB 5009.189-2023: National food safety standard - Determination of bongkrekic acid in foods
GB 5009.189-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Determination of
Bongkrekic Acid in Foods
ISSUED ON. SEPTEMBER 6, 2023
IMPLEMENTED ON. MARCH 6, 2024
Issued by. National Health Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword... 3
1 Scope... 4
Method I - Liquid Chromatography... 4
2 Principle... 4
3 Reagents and Materials... 4
4 Instruments and Equipment... 6
5 Analytical Procedures... 6
6 Result Calculation and Expression... 8
7 Precision... 9
8 Others... 9
Method II - Liquid Chromatography - Mass Spectrometry / Mass Spectrometry... 9
9 Principle... 9
10 Reagents and Materials... 9
11 Instruments and Equipment... 10
12 Analytical Procedures... 11
13 Result Calculation and Expression... 14
14 Precision... 14
15 Others... 14
Appendix A High Performance Liquid Chromatogram of Bongkrekic Acid Standard
Solution... 15
Appendix B Multiple Reaction Monitoring Mass Chromatogram of Bongkrekic Acid
Standard Solution... 16
National Food Safety Standard - Determination of Bongkrekic
Acid in Foods
1 Scope
This Standard specifies the methods for the determination of bongkrekic acid in foods.
In this Standard, Method 1 is applicable to the determination of bongkrekic acid in tremella
fungus and its products, fermented rice noodles and its products.
In this Standard, Method 2 is applicable to the determination of bongkrekic acid in tremella
fungus and its products, fungus and its products, cereals and its products.
Method I - Liquid Chromatography
2 Principle
The bongkrekic acid in the specimen is extracted by solvent, purified and concentrated by a
mixed strong anion exchange column or liquid-liquid extraction method. Adopt a high
performance liquid chromatograph for analysis and the external standard method for
quantitative determination.
3 Reagents and Materials
Unless it is otherwise specified, the reagents used in this Method are all analytically pure, and
the water is Grade-1 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Methanol (CH3OH). chromatographically pure.
3.1.2 Methanol (CH3OH).
3.1.3 Ammonia water (NH3 H2O). 25% ~ 28%.
3.1.4 Formic acid (CH2O2).
3.1.5 Hydrochloric acid (HCl).
3.1.6 Phosphoric acid (H3PO4).
3.1.7 Sodium bicarbonate (NaHCO3).
3.1.8 Petroleum ether (C5H12O2). with a boiling range of 30 C ~ 60 C.
3.1.9 Anhydrous ether (C4H10O).
3.1.10 Chloroform (CHCl3).
3.2 Preparation of Reagents
3.2.1 Phosphoric acid solution (45.4%). measure-take 45.4 mL of phosphoric acid, place it in a
100 mL volumetric flask, use water to dilute to a constant volume to the scale, and shake it well.
3.2.2 Sodium bicarbonate solution (40 g/L). weigh-take 40 g of sodium bicarbonate, add water
to dissolve it, transfer to a 1,000 mL volumetric flask, reach a constant volume to the scale, and
shake it well.
3.2.3 Hydrochloric acid solution (6 mol/L). measure-take 50 mL of hydrochloric acid, place it
in a 100 mL volumetric flask, add water to dilute to a constant volume to the scale, and shake
it well.
3.2.4 Ammonia water-methanol solution. measure-take 80 mL of methanol, add 1.0 mL of
ammonia water, add water to reach a constant volume of 100 mL, and shake it well.
3.2.5 Formic acid-methanol solution (2%). draw-take 2.0 mL of formic acid, add methanol to
100 mL, and shake it well.
3.2.6 Formic acid aqueous solution (pH 2.5). use formic acid to adjust the pH of water to 2.5
0.1, and shake it well.
3.3 Reference Material
Bongkrekic acid (C28H38O7, CAS. 11076-19-0). purity 95%, or a standard substance certified
by the state and awarded a reference material certificate.
NOTE. the reference material may use commercial standard solutions that satisfy the traceability
requirements.
3.4 Preparation of Standard Solutions
3.4.1 Bongkrekic acid standard stock solution (0.1 mg/mL). accurately weigh-take 10.0 mg
(accurate to 0.01 mg) of bongkrekic acid reference material, use methanol to dissolve it, transfer
to a 100 mL volumetric flask, and use methanol to reach a constant volume to the scale. Store
it in a 20 C refrigerator away from light. It shall remain valid for 6 months.
3.4.2 Bongkrekic acid standard series of working solutions. respectively and accurately draw-
take bongkrekic acid standard stock solution and use methanol to dilute it to a constant volume.
Thus, standard working solutions respectively with a mass concentration of bongkrekic acid of
Use a medium-speed filter paper to filter it, transfer the filtrate to the same 100 mL volumetric
flask, and use ammonia water-methanol solution to reach a constant volume to the scale, and
evenly mix it. Accurately measure-take 50.0 mL of the extracting solution, place it in 80 C
water bath and concentrate to about 3 mL by rotary evaporation, and reserve it for purification.
5.2.2 Specimen purification
Transfer all the concentrated specimen to the activated solid phase extraction column,
successively use 5 mL of water and 5 mL of methanol to rinse it and discard the effluent. Then,
use 6 mL of formic acid-methanol solution (2%) to elute it, collect the eluent; in 40 C water
bath, use nitrogen to blow it to dryness. Accurately add 0.5 mL of methanol, vortex to dissolve
it, evenly mix it, filter it through a 0.45 m microporous organic filter membrane, and reserve
it for later use.
5.3 Liquid-liquid Extraction Method
5.3.1 Specimen extraction
Weigh-take 20 g (accurate to 0.01 g) of specimen and place it in a conical flask. Add about 20
mL of methanol and soak it at room temperature in the dark for 1 hour. Then, add about 70 mL
of chloroform and 0.2 mL of phosphoric acid solution (45.4%), oscillate for 30 min, filter it,
transfer the filtrate to a 100 mL volumetric flask, and use chloroform to reach a constant volume
to the scale, evenly mix it. Accurately measure-take 50.0 mL of the filtrate and reserve it for
extraction.
5.3.2 Specimen extraction
Transfer the above-mentioned filtrate into a 150 mL separatory funnel, add sodium bicarbonate
solution (40 g/L) that has an equivalent volume with the filtrate, shake it for 2 minutes, and let
it stand for stratification. Then, take out the lower layer and place it in another separatory funnel.
Use 10 mL of sodium bicarbonate solution (40 g/L) to repeat the extraction twice, and gently
shake it. Combine the sodium bicarbonate solutions extracted in three times, add 25 mL of
chloroform, shake for 2 minutes and let it stand for stratification. Then, discard the chloroform
and slowly add hydrochloric acid solution (6 mol/L) into the separatory funnel, adjust the pH
of the solution to 2 ~ 3, add 50 mL of petroleum ether, shake it for 3 minutes, let it stand for
stratification, and take out the petroleum ether layer and place it in a rotary evaporator. Then,
respectively use 30 mL and 20 mL of petroleum ether to perform the extraction once and
combine the petroleum ether layer into the same bottle. In 40 C water bath, evaporate and
concentrate it to dryness; use a small amount of methanol to dissolve the extract in the rotary
evaporation bottle in several times and transfer it to a 5.00 mL glass centrifuge tube or
concentration bottle. At 40 C, blow nitrogen to concentrate it to dryness; accurately add 0.5
mL of methanol, vortex to dissolve it, evenly mix it, filter it through a 0.45 m microporous
organic filter membrane and reserve it for lat...
Get QUOTATION in 1-minute: Click GB 5009.189-2023
Historical versions: GB 5009.189-2023
Preview True-PDF (Reload/Scroll if blank)
GB 5009.189-2023: National food safety standard - Determination of bongkrekic acid in foods
GB 5009.189-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Determination of
Bongkrekic Acid in Foods
ISSUED ON. SEPTEMBER 6, 2023
IMPLEMENTED ON. MARCH 6, 2024
Issued by. National Health Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword... 3
1 Scope... 4
Method I - Liquid Chromatography... 4
2 Principle... 4
3 Reagents and Materials... 4
4 Instruments and Equipment... 6
5 Analytical Procedures... 6
6 Result Calculation and Expression... 8
7 Precision... 9
8 Others... 9
Method II - Liquid Chromatography - Mass Spectrometry / Mass Spectrometry... 9
9 Principle... 9
10 Reagents and Materials... 9
11 Instruments and Equipment... 10
12 Analytical Procedures... 11
13 Result Calculation and Expression... 14
14 Precision... 14
15 Others... 14
Appendix A High Performance Liquid Chromatogram of Bongkrekic Acid Standard
Solution... 15
Appendix B Multiple Reaction Monitoring Mass Chromatogram of Bongkrekic Acid
Standard Solution... 16
National Food Safety Standard - Determination of Bongkrekic
Acid in Foods
1 Scope
This Standard specifies the methods for the determination of bongkrekic acid in foods.
In this Standard, Method 1 is applicable to the determination of bongkrekic acid in tremella
fungus and its products, fermented rice noodles and its products.
In this Standard, Method 2 is applicable to the determination of bongkrekic acid in tremella
fungus and its products, fungus and its products, cereals and its products.
Method I - Liquid Chromatography
2 Principle
The bongkrekic acid in the specimen is extracted by solvent, purified and concentrated by a
mixed strong anion exchange column or liquid-liquid extraction method. Adopt a high
performance liquid chromatograph for analysis and the external standard method for
quantitative determination.
3 Reagents and Materials
Unless it is otherwise specified, the reagents used in this Method are all analytically pure, and
the water is Grade-1 water specified in GB/T 6682.
3.1 Reagents
3.1.1 Methanol (CH3OH). chromatographically pure.
3.1.2 Methanol (CH3OH).
3.1.3 Ammonia water (NH3 H2O). 25% ~ 28%.
3.1.4 Formic acid (CH2O2).
3.1.5 Hydrochloric acid (HCl).
3.1.6 Phosphoric acid (H3PO4).
3.1.7 Sodium bicarbonate (NaHCO3).
3.1.8 Petroleum ether (C5H12O2). with a boiling range of 30 C ~ 60 C.
3.1.9 Anhydrous ether (C4H10O).
3.1.10 Chloroform (CHCl3).
3.2 Preparation of Reagents
3.2.1 Phosphoric acid solution (45.4%). measure-take 45.4 mL of phosphoric acid, place it in a
100 mL volumetric flask, use water to dilute to a constant volume to the scale, and shake it well.
3.2.2 Sodium bicarbonate solution (40 g/L). weigh-take 40 g of sodium bicarbonate, add water
to dissolve it, transfer to a 1,000 mL volumetric flask, reach a constant volume to the scale, and
shake it well.
3.2.3 Hydrochloric acid solution (6 mol/L). measure-take 50 mL of hydrochloric acid, place it
in a 100 mL volumetric flask, add water to dilute to a constant volume to the scale, and shake
it well.
3.2.4 Ammonia water-methanol solution. measure-take 80 mL of methanol, add 1.0 mL of
ammonia water, add water to reach a constant volume of 100 mL, and shake it well.
3.2.5 Formic acid-methanol solution (2%). draw-take 2.0 mL of formic acid, add methanol to
100 mL, and shake it well.
3.2.6 Formic acid aqueous solution (pH 2.5). use formic acid to adjust the pH of water to 2.5
0.1, and shake it well.
3.3 Reference Material
Bongkrekic acid (C28H38O7, CAS. 11076-19-0). purity 95%, or a standard substance certified
by the state and awarded a reference material certificate.
NOTE. the reference material may use commercial standard solutions that satisfy the traceability
requirements.
3.4 Preparation of Standard Solutions
3.4.1 Bongkrekic acid standard stock solution (0.1 mg/mL). accurately weigh-take 10.0 mg
(accurate to 0.01 mg) of bongkrekic acid reference material, use methanol to dissolve it, transfer
to a 100 mL volumetric flask, and use methanol to reach a constant volume to the scale. Store
it in a 20 C refrigerator away from light. It shall remain valid for 6 months.
3.4.2 Bongkrekic acid standard series of working solutions. respectively and accurately draw-
take bongkrekic acid standard stock solution and use methanol to dilute it to a constant volume.
Thus, standard working solutions respectively with a mass concentration of bongkrekic acid of
Use a medium-speed filter paper to filter it, transfer the filtrate to the same 100 mL volumetric
flask, and use ammonia water-methanol solution to reach a constant volume to the scale, and
evenly mix it. Accurately measure-take 50.0 mL of the extracting solution, place it in 80 C
water bath and concentrate to about 3 mL by rotary evaporation, and reserve it for purification.
5.2.2 Specimen purification
Transfer all the concentrated specimen to the activated solid phase extraction column,
successively use 5 mL of water and 5 mL of methanol to rinse it and discard the effluent. Then,
use 6 mL of formic acid-methanol solution (2%) to elute it, collect the eluent; in 40 C water
bath, use nitrogen to blow it to dryness. Accurately add 0.5 mL of methanol, vortex to dissolve
it, evenly mix it, filter it through a 0.45 m microporous organic filter membrane, and reserve
it for later use.
5.3 Liquid-liquid Extraction Method
5.3.1 Specimen extraction
Weigh-take 20 g (accurate to 0.01 g) of specimen and place it in a conical flask. Add about 20
mL of methanol and soak it at room temperature in the dark for 1 hour. Then, add about 70 mL
of chloroform and 0.2 mL of phosphoric acid solution (45.4%), oscillate for 30 min, filter it,
transfer the filtrate to a 100 mL volumetric flask, and use chloroform to reach a constant volume
to the scale, evenly mix it. Accurately measure-take 50.0 mL of the filtrate and reserve it for
extraction.
5.3.2 Specimen extraction
Transfer the above-mentioned filtrate into a 150 mL separatory funnel, add sodium bicarbonate
solution (40 g/L) that has an equivalent volume with the filtrate, shake it for 2 minutes, and let
it stand for stratification. Then, take out the lower layer and place it in another separatory funnel.
Use 10 mL of sodium bicarbonate solution (40 g/L) to repeat the extraction twice, and gently
shake it. Combine the sodium bicarbonate solutions extracted in three times, add 25 mL of
chloroform, shake for 2 minutes and let it stand for stratification. Then, discard the chloroform
and slowly add hydrochloric acid solution (6 mol/L) into the separatory funnel, adjust the pH
of the solution to 2 ~ 3, add 50 mL of petroleum ether, shake it for 3 minutes, let it stand for
stratification, and take out the petroleum ether layer and place it in a rotary evaporator. Then,
respectively use 30 mL and 20 mL of petroleum ether to perform the extraction once and
combine the petroleum ether layer into the same bottle. In 40 C water bath, evaporate and
concentrate it to dryness; use a small amount of methanol to dissolve the extract in the rotary
evaporation bottle in several times and transfer it to a 5.00 mL glass centrifuge tube or
concentration bottle. At 40 C, blow nitrogen to concentrate it to dryness; accurately add 0.5
mL of methanol, vortex to dissolve it, evenly mix it, filter it through a 0.45 m microporous
organic filter membrane and reserve it for lat...
Share








