GB/T 5009.196-2003 Determination of inositol in health foods

This standard specifies the determination method of inositol in health foods. This standard is applicable to the determination of inositol as an effective ingredient added to tablets, capsules, beverages and other sample types. The detection limit of this method is 0.02μg, and the linear range is 0.1mg/mL~10mg/mL. GB/T 5009.196-2003 Determination of inositol in health foods GB/T5009.196-2003 Standard download decompression password: www.bzxz.net

ICS67.040
National Standard of the People's Republic of China
GB/T5009.196—2003
Determination of inositol in health foods
Determination of inositol in health foods2003-08-11Published
Ministry of Health of the People's Republic of China
National Administration of Standardization 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/T5009.196—2003
GB/T5009.196—2003
Inositol is a 6-carbon compound with 6 hydroxyl groups. It is a nutritional factor essential to humans and has been added to health foods as an effective ingredient. This method, which is based on the inositol test method of Taisho Pharmaceutical Co., Ltd. in Japan and combined with the existing instrument conditions in my country, provides a gas chromatography determination method for inositol in fortified nutrient tablets, capsules, and beverages. 552
1 Scope
Determination of inositol in health foods
This standard specifies the determination method for inositol in health foods. GB/T5009.196—2003
This standard is applicable to the determination of inositol as an effective ingredient added to tablets, capsules, beverages and other sample types. The detection limit of this method is 0.02#g, and the linear range is 0.1mg/mL~10mg/mL. 2 Principle
The solid sample extract or liquid sample dilution is concentrated to dryness, silanized, extracted with n-hexane, and qualitatively and quantitatively detected by gas chromatography hydrogen flame detector.
3 Reagents
3.1 Anhydrous ethanol.
3.2 n-hexane. bzxz.net
3.3 Anhydrous sodium sulfate.
3.4 ​​Trimethylsilyl chloride.
3.5 Hexamethyldisilazane.
3.6 Dimethylformamide.
3.7 Inositol standard solution: Dry the inositol standard (purity 99%) at 100℃±5℃ for 4h, accurately weigh 0.0500g, dissolve it in 70% ethanol solution, and accurately prepare 100.0mL solution. This solution contains 0.500mg inositol per mL. 3.8 Silylation reagent: Mix trimethylsilyl chloride, hexamethyldisilazane, and dimethylformamide in a volume ratio of 1:2:8, and prepare it before use.
4 Instruments
4.1 Gas chromatograph: with hydrogen flame detector (FID). 4.2 Rotary evaporator.
4.3 Ultrasonic cleaner.
5 Analysis steps
5.1 Sample pretreatment
5.1.1 Grind or mix 20 tablets or capsules, weigh a certain amount (accurate to 0.001g) in a test tube, add 70% ethanol solution to make the concentration about 0.5mg inositol per milliliter, extract by ultrasonic for 10min, centrifuge at 3000r/min for 5min, and keep the supernatant for later use. If the concentration of liquid sample is too high, dilute it with 70% ethanol solution to 0.5mg inositol per milliliter. 5.1.2 Accurately measure 1.0mL of sample solution (5.1.1) in the rotary evaporator concentration bottle, add 5mL of anhydrous ethanol, concentrate on the rotary evaporator at 60℃ until a small amount of liquid remains, and then add 5mL of anhydrous ethanol each time until the liquid in the concentration bottle is completely removed. 5.1.3 Accurately add 5.0mL of silanization reagent to the concentration bottle, and use ultrasonic vibration to completely disperse the contents in the bottle. Then place it in a 70℃ water bath and heat it for 10min. After cooling, add 10mL of water, then accurately add 3.0mL of n-hexane, shake for 1min and let it stand for 10min, centrifuge at a speed of 3000r/min for 5min, take out the n-hexane layer, add a small amount of anhydrous sodium sulfate, shake gently and let it stand, take the supernatant for sampling. Accurately measure 1.0mL of inositol standard solution (3.7) and operate according to 5.1.2 to obtain inositol standard derivative solution. 5.2 Gas chromatography reference conditions
5.2.1 Detector: FID.
GB/T5009.196—2003
5.2.2 Chromatographic column: BP525m×0.32mmi.d.) quartz elastic capillary column. 5.2.3
Gas flow rate: carrier gas (N2)
Tail gas (N2)
Split ratio
5.2.4 Column temperature: 190℃.
5.2.5 Inlet temperature: 245℃.
5.2.6 Attenuation: 4.
5.2.7 Paper speed: 2.
5.3 Chromatographic analysis
50mL/min
50mL/min
40mL/min
500mL/min
Measure 1aL of standard and sample derivative solution and inject them into the chromatograph. Use retention time for qualitative analysis and peak height or peak area of ​​sample for quantitative analysis compared with that of standard.
5.4 Chromatogram
Figure 1 Standard chromatogram of inositol
Figure 2 Sample chromatogram
Under the above chromatographic conditions, the retention time of inositol is 5.220min, and the concentration of inositol standard solution is 2.5mg/mL. 5.5 Preparation of standard curve
Prepare inositol standard solutions with concentrations of 0.1.0.5, 2.5.5.0, and 10.0mg/mL, perform gas chromatography analysis under given instrument conditions, and make a calibration curve using peak area versus concentration. 6 Result calculation
X_hXc×V100
Wherein:
X—Inositol content in the sample, in milligrams per hundred grams (or milligrams per hundred milliliters) [mg/100g (mL)]; hi
Sample peak height or peak area,
-Standard solution concentration, in milligrams per milliliter (mg/mL); V—Sample fixed volume, in milliliters (mL), h—Standard solution peak height or peak area;
-Sample volume, in grams (or milliliters) [g (or mL)]. The calculation result shall retain two significant figures.
7 Precision
The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10% of the arithmetic mean. 554
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