This standard specifies the method for determining the content of picolinic acid in health foods. This standard is applicable to the determination of the content of chromium picolinate added as an effective ingredient in tablets, capsules and other sample types. GB/T 5009.195-2003 Determination of chromium picolinate content in health foods GB/T5009.195-2003 Standard download decompression password: www.bzxz.net

ICS67.040
National Standard of the People's Republic of China
GB/T5009.195-2003www.bzxz.net
Determination of chromium picolinate in health foods2003-08-11Promulgated
Ministry of Health of the People's Republic of China
Standardization Administration of the People's Republic of China
2004-01-01Implementation
This standard is proposed and managed by the Ministry of Health of the People's Republic of China. This standard is drafted by the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. The main drafters of this standard are Yang Dajin, Fang Congrong and Wang Zhutian. GB/T5009.195—2003
GB/T5009.195-2003
Chromium picolinate is a stable compound formed by amino acid metabolite picolinic acid and trivalent chromium. It can pass through the cell membrane directly to act on tissue cells and has an important auxiliary effect on the treatment of diabetes. At present, chromium picolinate has been added to health foods as an effective ingredient. This method is developed based on the reference to the chromium picolinate detection method of Beijing Tangan Health Food Company and combined with the specific instrument conditions in my country. It is suitable for the determination of chromium picolinate in health foods such as tablets and capsules that add chromium picolinate. 546
1 Scope
Determination of chromium picolinate content in health foods This standard specifies the method for determining the content of chromium picolinate in health foods. GB/T5009.195—2003
This standard is applicable to the determination of chromium picolinate as an effective ingredient added to tablets, gels and other sample types. The detection limit of this method is 0.05pg, and the linear range is 2.00μg/mL~100pg/mL. 2 Principle
The crushed capsule and tablet samples are extracted and diluted with methanol decahydrate = 1+1, and the qualitative and quantitative detection is carried out according to the external standard method of HPLC UV detector.
3 Reagents
3.1 Methanol, high-grade purity.
3.2 Dipotassium hydrogen phosphate.
3.3 Potassium dihydrogen phosphate.
3.4 ​​Chromium picolinate standard solution: Accurately weigh 0.0100g of chromium picolinate standard, add methanol decahydrate = 1+1 and make up to 100.0mL. If there is a small amount of residue, use ultrasound to accelerate the dissolution. This solution contains 100μg chromium picolinate per milliliter. Instruments and equipment
4.1 High-performance liquid chromatograph: with UV detector. 4.2 Ultrasonic cleaner.
4.3 Centrifuge.
5 Analysis steps
5.1 Sample treatment
Take 20 tablets or capsules and crush or mix them. Weigh about 0.5g (accurate to 0.001g) of the sample into a graduated test tube, add methanol + water = 1+1 and make up to 20.0mL. After ultrasonic extraction for 5min, centrifuge at 3000r/min for 3min. Filter through a 0.45μm filter membrane and set aside.
5.2 Liquid chromatography reference conditions
5.2.1 Chromatographic column: μ-BONDAPAKTMCs4.6mm×250mm, 5um. 5.2.2 Column temperature: room temperature.
5.2.3 UV detector: detection wavelength 254nm. 5.2.4 Mobile phase: 0.125 mol/L phosphate buffer solution + acetonitrile = 425 + 755.2.5 Flow rate: 0.5 mL/min.
5.2.6 Injection volume: 10 μL.
5.3 Chromatographic analysis
Measure 10 μL of standard solution and sample solution and inject them into the chromatograph. The retention time is used for qualitative analysis and the peak height or peak area of ​​the sample is used for quantitative analysis compared with the standard.
GB/T5009.195-2003
5.4 Chromatogram
Under the above chromatographic conditions, the retention time of chromium picolinate is 7.023 and the concentration is 10 μg/mL. 5.5 Preparation of standard curve
Prepare standard solutions of chromium picolinate with concentrations of 2.00, 5.00, 10.0, 50.0, and 100ug/mL, perform liquid chromatography analysis under given instrument conditions, and draw a standard curve with peak height or peak area versus concentration. Calculation of results
Where:
hxc××100
hz×m×1000
-the content of chromium picolinate in the sample, in milligrams per hundred grams (mg/100g);-the peak height or peak area of ​​the sample,
-the concentration of the standard solution, in micrograms per milliliter (μg/mL); the volume of the sample, in milliliters (mL);-the peak height or peak area of ​​the standard solution;
-the mass of the sample, in grams (g).
The calculation result should retain two significant figures.
Precision
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 5% of the arithmetic mean. 548
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