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Method for determination of β-acetylpropionic acid in soy sauce
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SB/T 10417-2007
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PDF similar to SB/T 10417-2007
Basic data | Standard ID | SB/T 10417-2007 (SB/T10417-2007) | | Description (Translated English) | Method for determination of ��-acetylpropionic acid in soy sauce | | Sector / Industry | Domestic Trade Industry Standard (Recommended) | | Classification of Chinese Standard | X66 | | Classification of International Standard | 67.160 | | Word Count Estimation | 8,811 | | Date of Issue | 2007-01-25 | | Date of Implementation | 2007-07-01 | | Regulation (derived from) | ?Ministry of Commerce Announcement 2007 No.5 | | Issuing agency(ies) | Ministry of Commerce of the People's Republic of China | | Summary | This standard specifies the method for the determination of levulinic acid in soy sauce by gas chromatography. This standard applies to the determination of levulinic acid in soy sauce. The detection limit of the standard methods: 0. 010g/kg. |
SB/T 10417-2007: Method for determination of β-acetylpropionic acid in soy sauce---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Method for determination of β-acetylpropionic acid in soy sauce
ICS 67.160
X66
Record number..20182-2007
People's Republic of China domestic trade industry standard
Method for determination of levulinic acid in soy sauce
Released on.2007-01-25
2007-07-01 implementation
Published by the Ministry of Commerce
Content
Foreword III
1 Scope 1
2 Internal standard method 1
2.1 Principle 1
2.2 Reagents and solutions 1
2.3 Instruments and equipment 1
2.4 Analysis Step 1
3 External standard method 3
3.1 Principle 3
3.2 Reagent 3
3.3 Instruments and equipment 3
3.4 Analysis Step 3
Foreword
This standard is to comply with a series of new soy sauce standards issued by the state and industry, namely. GB 18186-2000 "making soy sauce",
SB 10336-2000 "Preparation of Soy Sauce", SB 10338-2000 "Acid Hydrolyzed Vegetable Protein Sauce" was formulated.
This standard was proposed by the China Condiment Association.
This standard is managed by the Ministry of Commerce of the People's Republic of China.
This standard was drafted. Beijing Food Brewing Research Institute, Guangdong Foshan Haitian Flavoring Food Co., Ltd.
The main drafters of this standard. Wu Ming, Zhong Fosheng, Huang Wenzhao, Che Yourong, Deng Yurong, Shi Yurong, Pan Shufen, Yang Guiju.
Method for determination of levulinic acid in soy sauce
1 Scope
This standard specifies the method for the determination of levulinic acid in soy sauce by gas chromatography.
This standard applies to the determination of levulinic acid in soy sauce.
The detection limit of this standard method. 0.010g/kg.
2 internal standard method
2.1 Principle
After acidification of the sample, levulinic acid was extracted with diethyl ether, and n-heptanoic acid was used as an internal standard substance, and gas phase color with a hydrogen flame ionization detector was used.
The spectrometer was measured and quantified by an internal standard method.
2.2 Reagents and solutions
Use analytically pure reagents and distilled or deionized water unless otherwise specified.
2.2.1 anhydrous sodium sulfate. burning at 650 ° C for 4 h, stored in a closed container for use.
2.2.2 Anhydrous ether.
2.2.3 Concentrated hydrochloric acid.
2.2.4 Saturated sodium chloride.
2.2.5 Standard product n-heptanoic acid. chromatographically pure, purity ≥99.5%.
2.2.6 Standard product levulinic acid. chromatographically pure, purity >98%.
2.2.7 n-heptanoic acid standard solution. Weigh 0.50g of n-heptanoic acid standard (accurate to 0.0001g) (2.2.5), and dilute with ethyl acetate to
100mL. The concentration of this standard solution was 0.0050 g/mL.
2.2.8 levulinic acid standard solution. Weigh 0.50g of levulinic acid standard (accurate to 0.0001g) (2.2.6), and make up with ethyl acetate
Up to 100mL. The concentration of this standard solution was 0.0050 g/mL.
2.2.9 Standard series solution. accurately absorb levulinic acid standard solution (2.2.8) 0.05mL, 0.1mL, 0.5mL, 1.0mL,
1.5 mL, 2.0 mL in 6 10 mL volumetric flasks, each adding 1.0 mL of normal heptanoic acid standard solution (2.2.7), and making up to volume with ethyl acetate.
That is, a standard series solution is equivalent to 25 μg, 50 μg, 250 μg, 500 μg, 750 μg, and 1000 μg of levulinic acid per ml.
2.3 Instruments and equipment
Laboratory routine instruments, equipment and the following.
2.3.1 100 mL stoppered test tube.
2.3.2 Gas Chromatograph. equipped with a hydrogen flame ionization detector (FID).
2.3.3 Column. Quartz elastic capillary column, column length 30m, inner diameter 0.25mm, coating thickness 0.5μm; fixing solution. Carbwax
20M. Or a column equivalent to this.
2.3.4 250 mL round bottom flask.
2.3.5 Concentration equipment (water bath, rotary evaporator or nitrogen blower).
2.4 Analysis steps
2.4.1 Sample extraction
Accurately weigh 5.0g sample (accurate to 0.0001g) in 100mL plugged test tube (2.3.1), add 10mL saturated sodium chloride solution
Liquid, 1.0 mL of normal heptanoic acid standard solution (2.2.7), concentrated hydrochloric acid 3.0 mL (2.2.3), shaken for 1 min, add 50.0 mL of anhydrous B
The ether was shaken and extracted for 3 min to 5 min, and allowed to stand for about 10 min to 15 min. After layering, draw the upper ether extract on a 250 mL round bottom.
In the flask (2.3.4), the extraction was repeated twice more, and the diethyl ether extract was combined, washed twice with 10 mL of a saturated sodium chloride solution, and the lower layer was discarded. B
The ether layer is dehydrated by excess sodium sulfate, concentrated to about dryness at about 45 ° C, and the residue is made up to 10 mL with ethyl acetate.
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