The main sampling method for the new Food Composition Database (FCD) is stratified sampling where units are taken from defined strata (subparts) of the parent population. 1) Example bread, 6 brands such as Gardenia, High 5, Mighty White, Restaurant Stall Restaurant Stall Restaurant Stall Restaurant Stall Restaurant Stall Restaurant Stall.
OBJECTIVE
SAMPLE CODING SYSTEM Category
Category sample
PROTOCOL FOR COLLECTION AND HANDLING OF RAW, PROCESSED AND PREPARED (FOOD AS CONSUMED) SAMPLES
State Code
Town Code
- SECTION 1: RAW AND PROCESSED FOODS
- SECTION 2: PREPARED FOODS
Atta for making capatti (Tepung atta untuk membuat capatti) Raw food of Brand 1, collected from Central Zone (Selangor). Alkaline destruction Loss of thiamine Avoid alkaline conditions and SO2 Light Photodegradation Loss of riboflavin Protect from light.
GENERAL PRECAUTIONARY MEASURES
Effects of sample storage and preparation on nutrient content and precautions required to minimize them
Type of food Grains and grain products Meat and meat products Starchy roots, tubers and products Eggs. Legumes and legume products Fish, shellfish and products Nuts, seeds and products Milk and milk products Vegetables and plant products Oils and fats.
Frozen Foods
Other details Any details the recorder considers relevant (eg after fresh samples are collected they are vacuum sealed) 4) Prepared (food as consumed) and Fast food. Other details Any details the recorder considers relevant (eg after fresh samples are collected they are vacuum sealed).
Receiving of Samples
Food products received from sampling points may require some simple preparations (e.g. washing and peeling or use immediately), while others may require detailed cooking instructions (e.g. chicken).
Identifying Sample
Preparation of Sample
Sample type Method of sample preparation Storage conditions Dry food/solid food. separately) except milk powder. First homogenize the solid part, then add the liquid part and use a spatula to mix and finally homogenize everything with a mixer.
Homogenizers
- Summary of method .1 Proximate
The composite laboratory analysis method is used to update the new Malaysian food composition database to ensure standardization and reliability of the data. The choice of the appropriate method under the quality assurance scheme is a crucial element to ensure the quality of the values in a food composition database.
LABORATORY METHODS OF ANALYSIS
Dry the container containing the sand, the glass rod and its lid in an oven at 105°C overnight and place in a desiccator to cool (about 30 min). After drying, use a pair of tongs to transfer the container and lid to the dryer to cool (about 45 min).
PROXIMATE
Transfer to desiccators to cool, then reweigh the dish and its contents. Transfer the dish to an oven and dry the sample at the prescribed temperature and time as in Table 4.
Standardization of hydrochloric acid 0.2N
Protein analysis
Vs and Vb = are sample and blank titration volumes (ml), S = sample weight (g) and 14 is the molecular weight of nitrogen N. Dry ashing procedures use a high-temperature muffle furnace capable of holding temperature between 500oC to 600oC.
Sample Preparation
Digestion
- Determination of Total Dietary Fiber
- Determination of Soluble Dietary Fiber
Proceed as for the determination of insoluble dietary fiber by instructing to combine the filtrate and water washings in prepared 600 ml tall beakers. Alternatively, adjust the weight of the combined solution of filtrate and wash water to 80 g by adding H2O and add 320 mL of 60 95% EtOH.
Extraction and analysis of sugars
- MINERALS
Evaluation of the acid digestion method with different solvent combinations for the determination of iron, zinc and lead in canned sardines. The organic material is first destroyed by dry ash, wet ash or microwave digestion method.
Digestion of sample
Determination
- FAT SOLUBLE VITAMINS
Cut open the 10 mg ampoule and make up to 100 mL with hexane to make a 100 µg/mL stock and store in amber bottles in the freezer. Cut open the 5 mg ampoule and make up to 25 mL with benzene to make a 200 µg/mL stock and store in amber bottles in the freezer.
Alkaline hydrolysis
Extraction
Instrument set up procedures
Turn the valve to the RUN position, remove the syringe from the low-pressure prime valve, and remember to turn the knob above the injector clockwise to allow mobile phase to flow through the column. Use the 715 software to open the mobile phase window and gradually increase the flow rate of the mobile phase to 2 mL/minute in 2 minutes.
Chromatography of carotenoids and retinol
v/v) Transfer 200 ml isopropanol into 1 liter volumetric flasks, dilute to the mark with dichloromethane and mix. e) Acetic acid solution - 10% - Transfer 10 ml of glacial acetic acid (AR grade) to a 100 ml volumetric flask, dilute to the mark with H2O and mix well. f) Ethanolic potassium hydroxide solution (KOH): Dissolve 140 g KOH pellets (AR grade) in 310 ml absolute ethanol and add 50 ml H2O. Prepare on the day of use. g) Mobile phase gradient mixture of acetonitrile, methanol and ethyl acetate. Note: Protect vitamin D2 and D3 standard solutions from high temperatures, oxygen and light to minimize degradation).
Preparation of Standard Mixture and Test Portions
Saponification and Extraction
Evaporation and solid-phase extraction
Calculations
Inject standard mixture into LC column at the beginning, middle and end of each series of test solutions. Where V1=volume of test portion, mL (usually 15); U= conversion factor to appropriate units (if necessary) and D = dilution factor for diluted powders or liquids.
System Suitability
The method for vitamins D2 and D3 is a reversed-phase HPLC procedure using a mixture of acetonitrile and methanol (75:25, v/v) as the mobile phase at a flow rate of 2.3 mL/min and a C18 column. Filter solvents through a 0.45 µm nylon membrane filter using the solvent filtration kit and degas with an ultrasonic bath.
Preparation of Sample
Extraction of food samples
HPLC conditions
Quantification of tocopherols and tocotrienols in Portuguese olive oils using HPLC with three different detection systems. Oils or fats (or unsaponifiable matter obtained from a processed product containing tocopherol esters) is dissolved in an organic solvent and subjected to direct high-performance liquid chromatography (HPLC) separation of individual tocopherols and tocotrienols.
Preparation of solutions of tocopherol standards (a) Alpha-tocopherol standard stock solution
Optimization of working parameters
Preparation of the test sample
The preparation of the test sample should, as far as practicable, be carried out in subdued lighting and in any case not in direct sunlight.
Preparation of the test solution
HPLC determination of tocopherols in the test solution
Number of determinations
- WATER SOLUBLE VITAMINS
These dried extracts can be kept in the dark for 3-5 days at <0ºC under N before LC analysis. Filter the mobile phase (Acetonitrile and deionized water) with 0.45 µm nylon membrane filter using solvent filtration apparatus daily before analysis.
Sample extraction
Turn off the pump, close the vent valve, set the required mobile phase composition (acetonitrile:water, 70:30) and a flow rate of 1 ml/min for thiamin and riboflavin analysis. Turn the pump back on and allow the column to equilibrate with the mobile phase, which typically takes 1 hour.
Chromatography of thiamine/ riboflavin
Set the pump to 100% at a flow rate of 5 mL/min to fill each channel in the solvent delivery system with the appropriate mobile phase for several minutes. Filter the mobile phase with a 0.45 µm nylon membrane filter using a solvent filter apparatus each day prior to analysis.
Sample Purification
Before turning on the HPLC, check the column, reservoir and mobile phase to ensure the correct column and mobile phase are being used. Set the required mobile phase composition (isocratic) and flow rate of 1 ml/min for niacin analysis.
Chromatography of niacin
Pantothenic acid (vitamin B5) is present in food in free form, as well as bound in coenzyme A (CoA) and acyl carrier protein (ACP). Therefore, liquid chromatography (LC) methods have been developed with post-column derivatization of pantothenic acid to a fluorescent compound - fluorescent 1-alkylthio-2-alkylisoindole.
Extract purification
Chromatography of Pantothenic Acid
Before turning on the HPLC, check the column, reservoir, and mobile phase to ensure that the correct column and mobile phase are being used. Set the required mobile phase composition (isocratic) and flow rate of 1 ml/min for vitamin B6 analysis.
Chromatography of Vitamin B6
Open the flush valve on the pump module by turning the knob a few turns counter-clockwise so that the solvent is later delivered directly to the waste container. The test based on the growth of Lactobacillus plantarum (biotin-dependent microorganism) according to the concentration of biotin in the medium.
Microbiological assay
Turn on the Agilent Chemstation control software and HPLC system, then warm up the instrument for at least 30 minutes before starting. Set the required composition of mobile phase (gradient) and flow rate of 0.4 ml/min for folic acid analysis.
Chromatography of folic acid
Prepare working solution (0.1 µg/ml) by pipetting 0.25 ml of stock solution (b) into 100 ml volumetric flask and make up to volume with deionized water. Quantitatively transfer the extract into a 50 mL volumetric flask, add internal standard, make up to volume with deionized water.
Instrument for set up procedures
Zero spectrophotometer at 505 nm against water and measure absorbance of standards (Astd), test solution (A'), blanks (Abl) and reagent blank (Areag). Guard column with I.D. of 2.1 mm, length of 5 mm and 1.7 µm which is packed with the same material as that of the analytical column.
Sample preparation
Ascorbic acid in sample is extracted in acidic environment and rapidly completed in subdued light. Note: Preparation of all standards for ascorbic acid should be carried out in a dimly lit room.
Instrument set up procedure
Set the pump to 100% with a flow rate of 5 ml/min to fill each channel with solvent. Turn off the pump, close the vent valve, set the required mobile phase composition (isocratic) and the flow rate of 1 ml/min for ascorbic acid analysis.
Chromatography of ascorbic acid
- AMINO ACIDS
Make sure the UV and visible lamps are turned on and set the DAD detector to a wavelength of 255 nm. The amino acid content in the food samples is detected and quantified using High Performance Liquid Chromatography (HPLC) with fluorescence detector equipped with Waters AccQTag amino acid analysis column and buffer.
Preparation of Eluent A
Preparation of Amino Acids Standard
Sample Preparation and Addition of Internal Standard
Preparation of MetO 2 (25 µmole/ml)
Preparation of cysteic acid (Cya) (25µmole/ml)
Preparation of Performic Acid
Sample Preparation
Preparation of Tryptophan Standard
Sample Preparation for Tryptophan
- FATTY ACIDS
Using the CRF obtained, calculate the concentration of each fatty acid in the test oil and finally report the concentration in % of the normalized weight using the following formula. Amount of each fatty acid = (Area x CRF) of each fatty acid in the test oil (WT.
Methylation methods for FAME
Condition of GCMS
- CHOLESTEROL
Standard 5a-cholestane available from Sigma Chemical Co., PO Box 14508, St. Table 1f Results of interlaboratory studies for the determination of cholesterol in foods by direct saponification methods. Before each reuse, clean the tubes with H2O, ethanol, hexane and acetone and dry them in an oven at 100 ºC.
Saponification
The HPLC method is intended for the simultaneous quantification of retinol, α-tocopherol and cholesterol in the hydrolyzate lipid fraction of shrimp waste. The detection is performed using two channels of a diode array spectrophotometer, 325 nm for retinol and 208 nm for α-tocopherol and cholesterol.
Saponification & Extraction
For the determination of retinol, α-tocopherol and cholesterol in the lipid fraction, the stock solution is in all cases analyzed together with the samples. Sanchez-Machado, D.I., and Rıos-Vazquez, N.J. High-performance liquid chromatography method for simultaneous quantification of retinol, α-tocopherol and cholesterol in shrimp waste hydrolyzate.
MANDATORY NUTRIENTS
- JAOAC 73, 849
8 Calcium, Ca Determination of minerals (calcium, sodium, magnesium and iron) in food products by ICP-OES after dry ashing. 9 Trans fatty acids Analysis of saturated, monounsaturated, polyunsaturated and trans fatty acids in food by GC.
FOOD LIST