GB 1886.105-2016 English PDF

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GB 1886.105-2016: National Food Safety Standard -- Food additives -- Pepper Orange
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GB 1886.105-2016	219	Add to Cart	3 days	National Food Safety Standard -- Food additives -- Pepper Orange	Valid

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Basic data

Standard ID: GB 1886.105-2016 (GB1886.105-2016)
Description (Translated English): National Food Safety Standard -- Food additives -- Pepper Orange
Sector / Industry: National Standard
Classification of Chinese Standard: X40
Word Count Estimation: 11,142
Date of Issue: 2016-08-31
Date of Implementation: 2017-01-01
Regulation (derived from): Announcement of the State Administration of Public Health and Family Planning 2016 No.11
Issuing agency(ies): National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

GB 1886.105-2016: National Food Safety Standard -- Food additives -- Pepper Orange

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
(Food safety national standard - Food additive - Pepper orange) National Standards of People's Republic of China National standards for food safety Food Additives Pepper Orange 2016-08-31 released 2017-01-01 Implementation People's Republic of China National Health and Family Planning Commission released National standards for food safety Food Additives Pepper Orange

1 Scope

This standard applies to the pepper peel and its products as raw materials, by extraction, filtration, concentration, succinate and other products made of food additives Pepper orange. 2 molecular formula, structural formula and relative molecular mass 2.1 Molecular formula Capsaicin. C40H56O3 Chrysanthemum. C40H56O4 2.2 Structural formula Capsaicin. Chrysanthemum. 2.3 Relative molecular mass Capsicumoids. 584.87 (according to.2007 International relative atomic mass) Chrysanthemum hemp. 600.87 (according to the.2007 international relative atomic mass)

3 technical requirements

3.1 sensory requirements Sensory requirements shall comply with the requirements of Table 1. Table 1 sensory requirements The project requires a test method Colorful orange or orange-red State oily liquid Take appropriate sample in a clean, dry, transparent glass tube Under light, observe the color and state 3.2 Physical and chemical indicators Physical and chemical indicators should be consistent with the provisions of Table 2. Table 2 Physical and chemical indicators Item Index Test Method The total amount of carotenoids, w /% is consistent with the assertion of A.3 in Appendix A. Pepper total alkaloid/(μg/mL) in accordance with claim A.4 in Appendix A. Capsaicin and pepper heme, w /% ≥ 30% of the total carotenoid content Appendix A A.5 Total Organic Solvent Residue/(mg/kg) ≤ 50 Appendix A A.6 Arsenic (As)/(mg/kg) ≤ 3.0 Appendix A A.7 Lead (Pb)/(mg/kg) ≤ 2.0 GB 5009.12 Note. Commercial pepper orange products should be in line with this standard pepper orange as raw material, can add edible dextrin, antioxidants and other accessories made.

Appendix A

Testing method A.1 General provisions The reagents and water used in this standard refer to the pure reagent and the tertiary water specified in GB/T 6682 when no other requirements are specified. test In the standard titration solution, impurity determination with the standard solution, preparation and products, in the absence of other requirements, according to GB/T 601, GB/T 602 and GB/T 603. The solution used in the test refers to the aqueous solution when it is not specified in the formulation of the solvent. A.2 Identification test A.2.1 Reagents and materials A.2.1.1 Sulfuric acid. A.2.1.2 Trichloromethane. A.2.1.3 Acetone. A.2.1.4 n-hexane. A.2.2 Identification method A.2.2.1 Color reaction Add 1 drop of 3 drops of trichloromethane and 1 drop of sulfuric acid to 1 drop of the sample. The solution was dark blue. A.2.2.2 Maximum absorption The sample was dissolved in acetone and had a maximum absorption peak at about 462 nm. The sample was dissolved in n-hexane and had a maximum at about 470 nm Absorption peak. A.3 Determination of total carotenoid content A.3.1 Methodological Summary Spectrophotometric method was used to determine the absorbance of carotenoids in pepper orange at the maximum absorption wavelength (about 462nm). content. A.3.2 Reagents and materials acetone. A.3.3 Instruments and equipment A.3.3.1 Spectrophotometer. A.3.3.2 Cuvette. 10mm. A.3.4 Analysis steps A.3.4.1 Preparation of sample solution Weigh 0.3g ~ 0.5g sample (accurate to 0.0002g), placed in 100mL volumetric flask, dissolved with acetone and diluted to the mark, standing 2min. Absorb 1mL of the solution, placed in another 100mL volumetric flask, fixed with acetone to the scale, full shake. A.3.4.2 Determination The sample solution was placed in a 10 mm cuvette and the absorbance A was read at the maximum absorption wavelength (about 462 nm). Adjust the sample concentration, So that the absorbance between 0.3 to 0.7. A.3.5 Calculation of results The mass fraction of carotenoids, w1, is calculated according to formula (A.1) w1 = A0 × 104 2100 × m1 (A.1) Where. A0 --- absorbance value of sample solution; 104 - dilution factor of sample solution; 2100 --- Percent Absorption Coefficient of Pepper Red/Pepper Rutin at 462nm in Acetone E1 m; m1 --- the quality of the sample, in grams (g). The result of the calculation indicates one after the decimal point. A.4 Determination of total alkaloids in peppers A.4.1 Methodological Summary Determination of total alkaloids of pepper (reduced dihydrocapsaicin, capsaicin and dihydro capsaicin) by high performance liquid chromatography. A.4.2 Reagents and materials A.4.2.1 Ethanol. A.4.2.2 Acetone. A.4.2.3 acetonitrile. A.4.2.4 Acetic acid solution. 1 99. A.4.2.5 Synthetic capsaicin standard, purity ≥99%. A.4.3 Instruments and equipment A.4.3.1 High performance liquid chromatograph. with 20 μL dosing ring, equipped with fluorescence detector or UV detector. A.4.3.2 Solid phase extraction cartridge. Sep-PAKC186mL, or other equivalent solid phase extraction cartridge. A.4.4 Reference chromatographic conditions A.4.4.1 Column. C18 stainless steel column, 150 mm x 4.6 mm, particle size 5 m, or other equivalent column. A.4.4.2 Mobile phase. acetonitrile. acetic acid solution = 40.60. A.4.4.3 Mobile phase flow rate. 1.5 mL/min. A.4.4.4 Detection wavelength. Fluorescence detector excitation wavelength 280nm, emission wavelength 325nm; UV detector detection wavelength 280nm. A.4.4.5 Injection volume. 20 μL. A.4.5 Analysis steps A.4.5.1 Preparation of standard solutions Weigh 75mg synthetic capsaicin standard, accurate to 0.01mg, placed in 500mL volumetric flask, diluted with ethanol diluted to the mark, Shake, the solution for the standard solution A (mass concentration of 150μg/mL). Absorb 10mL standard solution A, placed in 100mL volumetric flask , Diluted with ethanol to the mark, shake, the solution for the standard solution B (mass concentration of 15μg/mL). Draw 5mL standard solution B, placed in a 100mL volumetric flask, diluted with ethanol to the mark, shake, the solution for the standard solution C (mass concentration of 0.75μg/mL). A.4.5.2 Preparation of sample solution Weigh 5g sample, accurate to 0.0001g, placed in 50mL volumetric flask, to avoid the sample stick to the volumetric flask wall. Add 5mL Acetone, shake until the sample is completely dissolved. Tilt the 45 ° angle to see if the specimen is attached to the bottom of the bottle. Slowly add ethanol (95% or absolute ethanol) Until the solution is turbid, diluted to the scale, mixed evenly. Use a 10 mL syringe to draw 5 mL of the sample solution directly to a size of 6 mL In the solid phase extraction column, the sample is allowed to adhere to the inner wall of the syringe. The sample was passed through a column and collected in a 25 mL volumetric flask. use 5mL ethanol wash the extraction column, washed three times, the washing liquid collected to the volumetric flask, with ethanol constant volume to the scale, through the 0.45μm filter Filter, the filtrate into the glass bottle. A.4.5.3 Determination Under the conditions of A.4.4 reference chromatography, the sample solution and standard solution were chromatographed respectively. Record the sample solution in the chromatogram The peak area of the capsaicin, the peak area of the capsaicin, the peak area of the dihydrocapsaicin, and the standard of the standard solution Peak area AS. A.4.6 Calculation of results The concentration of ρN, in micrograms per milliliter (μg/mL), is calculated according to formula (A.2) ρN = AN AS × ρS × rN (A.2) Where. AN - the average peak area of dihydrolipid base; AS --- the average peak area of the standard; ρS --- Mass concentration of standard solution in micrograms per milliliter (μg/mL); The response factor of rN - reduced dihydrocapsin relative standard. The mass concentration of capsaicin is in ρC, expressed in micrograms per milliliter (μg/mL), calculated according to formula (A.3) ρC = AC AS × ρS × rC (A.3) Where. AC - the average peak area of capsaicin; AS --- the average peak area of the standard; ρS --- Mass concentration of standard solution in micrograms per milliliter (μg/mL); rC --- capsaicin relative to the standard response factor. The mass concentration ρD of dihydro capsaicin is in micrograms per milliliter (μg/mL) calculated according to formula (A.4) ρD = AD AS × ρS × rD (A.4) Where. AD --- the average peak area of dihydrolipid base; AS --- the average peak area of the standard; ρS --- Mass concentration of standard solution in micrograms per milliliter (μg/mL); rD --- Dihydroliparin base relative to the standard response factor. The mass concentration ρ of the total capsaicin (reduced dihydrocapsaicin, capsaicin and dihydro capsaicin) in the sample is in micrograms per milliliter (μg/mL), calculated according to formula (A.5). ρ = ρN ρC ρD (A.5) Where. The mass concentration of ρN --- reduced dihydrocapsa alkaloids in micrograms per milliliter (μg/mL); ρC --- the mass concentration of capsaicin in micrograms per milliliter (μg/mL); The mass concentration of ρD --- dihydro capsaicin is in micrograms per milliliter (μg/mL). The parameters of capsaicin are shown in Table A.1. Table A.1 capsaicin parameters name UV detector response factor (UV) Fluorescence detector response factor (FLU) Relative retention time Lower dihydrocapsa (rN) 0.98 0.92 0.90 Capsaicin (rC) 0.89 0.88 1.00 Dihydrocarsticin (rD) 0.93 0.93 1.58 Determination of heparin and pepper A.5.1 Methodological Summary The contents of capsaicin and chrysanthemum were determined by area normalization method by high performance liquid chromatography (HPLC). A.5.2 Reagents and materials A.5.2.1 anhydrous sodium sulfate. A.5.2.2 Acetone. Chromatographic pure. A.5.2.3 Ethyl ether. A.5.2.4 Potassium hydroxide - methanol solution. 2 g of potassium hydroxide dissolved in 100 mL of methanol. A.5.3 Instruments and equipment High Performance Liquid Chromatograph. with a diode array detector, the spectral range of 350nm ~ 600nm. A.5.4 Reference chromatographic conditions A.5.4.1 Column. Stainless steel column with a length of 250 mm and an inner diameter of 4 mm. The stationary phase is C18, or other equivalent column. A.5.4.2 Detection wavelength. 450 nm. A.5.4.3 Flow rate. 1.5 mL/min. A.5.4.4 Injection volume. 5 μL. A.5.4.5 Gradient elution. see Table A.2. Table A.2 Gradient elution procedures Time/min acetone /% water /% -10 (before injection) 75 25 A.5.5 Analysis steps A.5.5.1 Preparation of sample solution Weigh 0.2g sample, accurate to 0.01mg, dissolved in the amount of acetone, transferred to 500mL separatory funnel, adding acetone to the solution volume For 100mL, then add 100mL ether, mix well, filter. Add 100mL potassium hydroxide - methanol solution, put it aside for 1h, shake regularly move. The aqueous phase was removed and the organic phase was washed with water several times until the washings were colorless. Filtered through anhydrous sodium sulphate and evaporated at 35 ° C with a rotary evaporator dry. The dried pigment was transferred to a 25 mL volumetric flask, dissolved in acetone, and allowed to cool. Can be used before the analysis with an ultrasonic generator The product was sufficiently dissolved and filtered through a 0.45 μm filter. A.5.5.2 Determination Under the reference chromatographic conditions of A.5.4, the sample solution was chromatographed to determine the capsules in the sample solution chromatogram and chili The peak area of capsaicin and chrysanthemum in the sample chromatogram was recorded, and the area of the capsaicin was calculated by area normalization method. And the content of chrysanthemum. Peak sequence. new lutein, chrysanthemum, yellow, chrysanthemum, oxidized zeaxanthin, carrots Yellow pigment A, hidden pepper quality, β-zeaxanthin, β-carotene. A.5.6 Calculation of results The quality fraction w2 of capsaicin and chrysanthemum is calculated according to formula (A.6). w2 = A1 A2 ΣAi × 100% (A.6) Where. A1 - peak area of capsaicin in sample; A2 - peak area of capsaicin in the sample; ΣAi --- the sum of the peak areas of each component i in the sample. The result of the calculation indicates one after the decimal point. A.6 Determination of total organic solvent residues A.6.1 Methodological summary The total organic solvent (ethyl acetate, ethanol, acetone, 2-propanol, hexane) was determined by internal standard method using gas chromatography. A.6.2 Reagents and materials A.6.2.1 Methanol. A.6.2.2 Internal standard. 3-methyl-2-pentanone. A.6.2.3 Ethyl acetate. A.6.2.4 Ethanol. A.6.2.5 Acetone. A.6.2.6 2-propanol. A.6.2.7 Hexane. A.6.3 Instruments and equipment Gas chromatograph. equipped with hydrogen flame ionization detector. A.6.4 Reference chromatographic conditions A.6.4.1 Column. quartz capillary column, length 30m, diameter 0.53mm, film thickness of 1μm (such as DB-1 or can reach the same From the effect of other capillary columns). A.6.4.2 Carrier gas. helium. A.6.4.3 Flow rate. 5 mL/min. A.6.4.4 Gasification chamber temperature. 140 ° C. A.6.4.5 Detector temperature. 300 ° C. A.6.4.6 Column temperature. 35 ° C for 5 min, then raised to 90 ° C at 5 ° C/min for 6 min. A.6.4.7 Injection volume. 1 μL to 2 μL. A.6.5 Analysis steps A.6.5.1 Preparation of internal standard solutions Measure 50.0 mL of methanol accurately, add to a 50 mL vial, seal, weigh, and then inject 15 [mu] L of 3-methyl-2- Pentanone, weighed, accurate to 0.01mg. A.6.5.2 Preparation of sample solution Weigh 0.20g sample, accurate to 0.1mg, add to 50mL vials, then add 5.0mL methanol and 1.0mL internal standard solution Liquid, heated at 60 ° C for 10 min, fully shaken for 10 s. A.6.5.3 Preparation of standard curve solutions A.6.5.3.1 Preparation of standard stock solutions Accurately measure 50.0 mL of methanol, add to 50 mL vials and seal. Accurate weighing, accurate to 0.01mg. Through the septum Into the 50μL standard (target compound), weighing, mixing evenly. A.6.5.3.2 Preparation of standard use solutions Accurately remove 1 mL of the standard stock solution, add to the 50 mL vial, and then add 4.0 mL of methanol, mix well. A.6.5.3.3 Drawing of standard curves Accurately take 0mL, 0.1mL, 0.2mL, 0.3mL, 0.5mL standard solution, add to 50mL vials, and then accurate Add 5 mL, 4.9 mL, 4.8 mL, 4.7 mL, 4.5 mL methanol and 1.0 mL internal standard solution and mix well. In A.6.4 reference column The ratio of the peak area of each component to the peak area of the internal standard was taken as the ordinate, and the standard curve was plotted with the concentration of each component as the abscissa. A.6.5.4 Determination The sample solution was chromatographed under A.6.4 reference chromatography. The peak area of each component and the peak of the internal standard were obtained according to the chromatogram And then calculate the concentration of each component in the sample according to the standard curve. A.6.6 Calculation of results The mass fraction wi of the residue in the organic solvent (ethyl acetate, ethanol, acetone, 2-propanol, hexane) in the sample is in milligrams per thousand Gram (mg/kg), calculated according to formula (A.7). wi = ρ i × V × 1000 mi (A.7) Where. ρi --- mass concentration of each component in the sample, in milligrams per milliliter (mg/mL); V --- the total volume of the sample solution in milliliters (mL); 1000 --- conversion factor; mi --- the quality of the sample, in grams (g). The residual amount of each organic solvent (ethyl acetate, ethanol, acetone, 2-propanol, hexane) was calculated from the formula (A.7), and the residual amount of each component And the sum of the total organic solvent residues in the sample. A.7 Determination of arsenic (As) A.7.1 Methodological Summary After the pepper orange was digested by wet method, the sample solution was prepared and the content of arsenic was determined by atomic absorption spectrometry. A.7.2 Reagents and materials A.7.2.1 Nitric acid. A.7.2.2 Sulfuric acid solution. 1 1. A.7.2.3 Nitric acid - Perchloric acid mixed solution. 3 1. A.7.2.4 Hydrochloric acid solution. 1 10. A.7.2.5 Sodium hydroxide solution. 1 g/L. A.7.2.6 Sodium borohydride solution. 8 g/L. Weigh 8g sodium borohydride, dissolved in the amount of 1g/L sodium hydroxide solution, diluted to 1000mL. A.7.2.7 Potassium iodide solution..200 g/L. A.7.2.8 arsenic (As) standard solution. according to GB/T 602 preparation and calibration, and then according to the requirements of the instrument used to dilute the preparation of arsenic The corresponding concentration of the three standard solution. A.7.3 Instruments and equipment Atomic Absorption Spectrometer. A.7.4 Reference chromatographic conditions A.7.4.1 Arsenic hollow cathode lamp analysis line Wavelength. 193.7nm; Slit. 0.5nm ~ 1.0nm; Lamp current. 6mA ~ 10mA. A.7.4.2 Carrier gas flow rate. argon 250 mL/min. A.7.4.3 Atomizer temperature. 900 ° C. A.7.5 Analysis steps A.7.5.1 Sample digestion Approximately 1 g of sample (accurate to 0.001 g) was weighed and placed in a 250 mL triangular or round bottom flask with 10 mL to 15 mL of nitric acid and 2mL sulfuric acid solution, shake and heat with a small fire out of the nitrogen dioxide gas, the solution becomes brown, stop heating, let cool after adding 5mL of nitrate Acid - perchloric acid mixture, strong fire heated to the solution transparent or slightly yellow, such as still opaque, put cold and then add 5mL nitric acid - perchloric acid mixed solution Liquid, continue to heat to the solution transparent colorless or yellowish and produce white smoke (to avoid the phenomenon of carbonization occurs dry), stop heating, let cool and add 5mL Water heated to boiling, remove the residual nitric acid - perchloric acid (if necessary, add water to boil again), continue to heat to white smoke, keep 10min, After cooling into the 100mL volumetric flask (if the solution appears turbidity, precipitation or mechanical impurities to be filtered), diluted with hydrochloric acid solution volume, as a test Sample solution. While preparing a blank solution. A.7.5.2 Determination Measure 25mL of the digested sample solution to 50mL volumetric flask, add 5mL potassium iodide solution, diluted with hydrochloric acid solution volume, shake And allowed to stand for 15 min as a test solution for the sample. At the same time remove the arsenic standard solution in the same way to volume to 50mL volumetric flask, while the blank solution prepared blank test solution. A.7.6 Calculation of results The mass fraction w3 of arsenic (As) in milligrams per kilogram (mg/kg) is calculated according to formula (A.8) w3 = (m3-m2) x 1000 m4 × (A.8) Where. m3 --- According to the standard curve to calculate the quality of the sample solution, in milligrams (mg); m2 --- Calculate the mass of the blank solution in milligrams (mg) according to the standard curve; 1000 --- conversion factor; m4 --- the quality of the sample, in grams (g); 25 - the volume consumed by the sample in milliliters (mL); 100 --- volume of sample volume, in milliliters (mL). The absolute difference between the parallel determination results is not more than 0.1 mg/kg, and the arithmetic mean is taken as the measurement result. 6102- 501 􀏕 6881 ......

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