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GB/T 22246-2008 English PDF (GBT22246-2008)

GB/T 22246-2008 English PDF (GBT22246-2008)

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GB/T 22246-2008: Determination of calcium pantothenate in health foods

This Standard specifies the determination method of calcium pantothenate in the nutrient supplements types of health foods. This Standard is applicable to determination of calcium pantothenate in the nutrient supplements types of health foods.
GB/T 22246-2008
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 67.040
C 53
Determination of Calcium Pantothenate in
Health Foods
ISSUED ON. JULY 31, 2008
IMPLEMENTED ON. NOVEMBER 1, 2008
Issued by. Ministry of Health of PRC; Standardization Administration of China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principles ... 4
3 Reagents and Materials ... 4
4 Apparatuses and Instruments ... 5
5 Analysis Steps ... 5
6 Calculation ... 6
7 Precision ... 7
8 Chromatograms ... 7
Foreword
This Standard was proposed by and shall be under the jurisdiction of Ministry of Health of PRC.
Drafting organizations of this Standard. Chinese Center for Disease Control and Prevention nutrition and food security.
Participating drafting organizations of this Standard. Hebei Provincial Center for Disease Control and Prevention.
Chief drafting staffs of this Standard. Yang Dajin, Fang Congrong, Ma Lan, Wang Zhutian, and Qin Zhenshun.
This Standard is first-time published.
Determination of Calcium Pantothenate in
Health Foods
1 Scope
This Standard specifies the determination method of calcium pantothenate in the nutrient supplements types of health foods.
This Standard is applicable to determination of calcium pantothenate in the nutrient supplements types of health foods.
This Standard?€?s Limit of Detection. when sampling amount is 1.0g, fix the volume to 25mL; when injection amount is 10??L, the Limit of Detection (LOD) is 2x10-4g/100g, and the Limit of Quantity (LOQ) is 6x10-4g/100g.
This Standard?€?s linear range. 2.5??g/mL ~ 80??g/mL.
2 Principles
According to calcium pantothenate?€?s physiochemical properties - it is soluble in water, it is unstable in acid and alkali, and it is very stable in neutral (pH=5.0~7.0) conditions - the calcium pantothenate in the specimen shall use water to extract under the ultrasonic oscillation; after fixed-volume and centrifugation, take supernatant filtration membrane; go through the separation of C18 reverse phase column; then detect at 200nm wave length of UV detector; identify the qualitative as per the chromatographic retention time; identify the quantification as per the external-standard method. 3 Reagents and Materials
3.1 Acetonitrile (CH3CN). chromatographic pure.
3.2 Phosphoric acid (H3PO4). analytical reagent.
3.3 Potassium dihydrogen phosphate (KH2PO4). analytical reagent.
3.4 0.02mol/L potassium dihydrogen phosphate solution. take 2.722g of
potassium dihydrogen phosphate; add water to dissolve into 1000mL; use
phosphoric acid to adjust the pH value to 3.0.
3.5 Water (H2O). Grade-1 lab water, conductivity (25??C) is 0.01mS/m.
3.6 Calcium pantothenate standard stock solution. weigh 0.1g of calcium pantothenate standard product (accurate to 0.0001g); place it in a 100mL flask; add water to dissolve; fix volume to graduation; mix evenly (keep in 4??C refrigerator for spare use; such solution can be stored for 5d).
3.7 Calcium pantothenate standard use solution. exactly weigh 1.0mL of standard stock solution (see Clause 3.6); place it in a 100mL flask; add water to dilute to graduation; mix evenly (keep in 4??C refrigerator for spare use; such solution can be stored for 5d).
4 Apparatuses and Instruments
4.1 High performance liquid chromatography instrument. attached with UV Detector. 4.2 Ultrasonic cleaner.
4.3 Centrifuge. 4000r/min.
5 Analysis Steps
5.1 Specimen preparation
5.1.1 Solid tablet or capsule specimens. weigh 0.1g~1.0g of post-pulverizing and uniform specimen (accurate to 0.001g); make the specimen concentration to be within the standard curve. Place the specimen into a 25mL flask; add 200mL of water; after conducting ultrasonic extraction for 20min, add water to the graduation; shake uniformly; after centrifugation, pass the supernatant through the 0.45??m membrane; the filtrate is to be injected.
5.1.2 Liquid specimen. except that, for carbonated drink, it needs ultrasound to remove the carbon dioxide before sampling - for other liquid samples, weigh directly and accurately the appropriate amount of sample-liquid; make the specimen concentration to be within the standard curve. Place the specimen into the 25mL flask; use water to dilute to the graduation, and then mix evenly; pass the specimen through 0.45??m membrane, and set aside filtrate.
5.2 Preparation of standard curve
Absorb 0.25, 0.50, 1.0, 2.0, 4.0, and 8.0 mL of calcium pantothenate standard use solution (equivalent to 2.5??g, 5.0??g, 10??g, 20??g, 40??g, and 80??g of calcium pantothenate), place them into 10mL flasks respectively, dilute with water to the graduation, and mix evenly. In the given instrument conditions, conduct

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