GB/T 5009.193-2003 Determination of dehydroepiandrosterone (DHEA) in health foods

This standard specifies the determination method of dehydroepiandrosterone (DHEA) in health foods. This standard is applicable to the determination of dehydroepiandrosterone (DHEA) added to tablets, capsules and other sample types. The detection limit of this method is 0.02μg, and the linear range is 0.0400mg/mL～10.0mg/mL. GB/T 5009.193-2003 Determination of dehydroepiandrosterone (DHEA) in health foods GB/T5009.193-2003 Standard download decompression password: www.bzxz.net

ICS67.040
National Standard of the People's Republic of China
GB/T5009.193-2003
Determination of dehydroepiandrosterone in health foods2003-08-11Published
Ministry of Health of the People's Republic of China
Standardization Administration of the People's Republic of Chinabzxz.net
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. Introduction
GB/T5009.193—2003
GB/T5009.193—2003
Dehydroepiandrosterone (DHEA) is a type of human adrenaline. It has certain effects on preventing and treating cardiovascular diseases, enhancing immunity, and delaying aging. It is not allowed to be added to health foods at present. In order to effectively supervise and detect this ingredient, this method provides a high-performance liquid chromatography determination method for dehydroepiandrosterone in tablet and capsule health foods based on reference to foreign literature.
1 Scope
GB/T5009.193—2003
Determination of dehydroepiandrosterone (DHEA) in health foods This standard specifies the determination method of dehydroepiandrosterone (DHEA) in health foods. This standard is applicable to the determination of dehydroepiandrosterone (DHEA) added to tablets, capsules and other sample types. The detection limit of this method is 0.02μg, and the linear range is 0.0400mg/mL~10.0mg/mL. 2 Principle
The crushed capsule and tablet samples are extracted and diluted with mobile phase, and qualitatively and quantitatively detected by high-performance liquid chromatography UV detector.
3 Reagents
Unless otherwise specified, the water used in the analysis is double distilled water. 3.1 Methanol, high-grade purity.
3.2 Dehydroepiandrosterone (DHEA) standard solution: Accurately weigh 0.0100g of dehydroepiandrosterone (DHEA) standard (purity ≥99.99%), add to the detection mobile phase and make up to 10mL. This solution contains 1mg dehydroepiandrosterone (DHEA) per milliliter. 4 Instruments
4.1 High-performance liquid chromatograph: with UV detector (UV). 4.2 Ultrasonic cleaner.
4.3 Centrifuge.
5 Analysis steps
5.1 Sample treatment
Take more than 20 tablets or capsules for grinding and mixing, weigh an appropriate amount of sample (accurate to 0.001g) in a volumetric flask, add mobile phase to make up to 10.0mL, so that the concentration is about 1mg of dehydroepiandrosterone (DHEA) per milliliter. Ultrasonic extraction for 5min, centrifuge at 3000r/min for 3min. Accurately take 2.0mL of sample solution in a test tube, add mobile phase to make up to 5.0mL, shake well. Filter through 0.45μm filter membrane and set aside.
5.2 Liquid chromatography reference conditions
5.2.1 Chromatographic column: μ-BONDAPAKTMCs4.6mmX250mm, 5μm. 5.2.2 Column room temperature.
5.2.3 UV detector: detection wavelength 215nm. Mobile phase: methanol + water = 80 + 20.
5.2.5 Flow rate: 0.6mL/min
5.2.6 Injection volume 10μL.
Chromatographic analysis: Take 10μL 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 5.2.7
Compare with the standard for quantitative analysis.
GB/T5009.193-2003
Chromatogram:
Figure 1 DHEA standard chromatogram
Figure 2 Sample chromatogram
Under the above chromatographic conditions, the retention time of dehydroepiandrosterone (DHEA) is 7.40min, and the concentration of the standard solution is 0.200mg/mL.
5.3 Preparation of standard curve
Prepare standard solutions of dehydroepiandrosterone (DHEA) with concentrations of 0.0400, 0.200.1.00, 5.00, and 10.0 mg/mL respectively, perform liquid chromatography analysis under given instrument conditions, and draw a standard curve based on peak height or peak area versus concentration. Calculation of results
XhiXcxVx5x100
h2XmX2
Wherein:
X—the content of dehydroepiandrosterone (DHEA) in a sample, in milligrams per hundred grams (mg/100g); h.
—the peak height or peak area of ​​a sample;
—the concentration of a standard solution, in milligrams per liter (mg/mL); V—the volume of a sample, in milliliters (mL); h2-the peak height or peak area of ​​a standard solution;
the mass of a sample, in grams (g).
The calculation result shall 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, 536
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