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royal jelly
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GB 9697-2008
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PDF similar to GB 9697-2008
Basic data Standard ID | GB 9697-2008 (GB9697-2008) | Description (Translated English) | royal jelly | Sector / Industry | National Standard | Classification of Chinese Standard | B47 | Classification of International Standard | 65.140 | Word Count Estimation | 11,194 | Date of Issue | 2008-06-27 | Date of Implementation | 2009-01-01 | Older Standard (superseded by this standard) | GB/T 9697-2002 | Quoted Standard | GB/T 601; GB/T 5009.4-2003; GB 7718 | Regulation (derived from) | Announcement of Newly Approved National Standards No. 10 of 2008 (total 123) | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | Summary | This Chinese standard specifies the definition of royal jelly, grade, quality, test methods, packaging, labeling, storage and transport requirements. This standard applies to royal jelly production and trade. |
GB 9697-2008: royal jelly---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.
royal jelly
ICS 65.140
B47
National Standards of People's Republic of China
Replacing GB/T 9697-2002
Royal Jelly
Posted 2008-06-27
2009-01-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
Chapter 4 of this standard is mandatory, the rest are recommended.
This standard replaces GB/T 9697-2002 "royal jelly."
This standard compared with GB/T 9697-2002 The main changes are as follows.
--- By the recommended standards to the provisions of mandatory standards;
--- Increasing the terms and definitions;
--- Modify the definition of royal jelly;
--- Adjust the threshold value of protein content.
Appendix A of this standard is a normative appendix.
This standard is proposed and managed by China Federation of Supply and Marketing Cooperatives.
This standard was drafted. Nanjing Laoshan Pharmaceutical Co., Ltd., China Supply and Marketing Cooperatives bee products Standardization Technical Committee
Secretariat, the China Association of bee royal jelly professional committees.
The main drafters of this standard. Li Zijian, tube Chunhua, Li Xiaodong, Chenming Hu, Yang ice.
This standard replaces the standards previously issued as follows.
--- GB/T 9697-2002.
Royal Jelly
1 Scope
This standard specifies the definition of royal jelly, grade, quality, test methods, packaging, labeling, storage, transportation requirements.
This standard applies to the production and trade of royal jelly.
2 Normative references
The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research
Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.
Preparation of GB/T 601 chemical reagent standard titration solution
Determination of GB/T 5009.4-2003 ash in foods
GB 7718 pre-packaged food labels General
3 Terms and Definitions
The following terms and definitions apply to this standard.
3.1
Royal Jelly royaljely
Worker bees swallow gland and palate gland secretion, mainly used for feeding the queen bee and wasp larvae milky white, yellow or light orange syrupy substance.
4 Requirements
4.1 Sensory requirements
4.1.1 Color
Whether it is sticky paste state or frozen state should be white, yellow or light orange, shiny. There are ice crystals when frozen
luster.
4.1.2 Odour
When the sticky paste state, there should be similar to nectar or pollen of flavor and spice. Pure smell, without fermentation, rancid odor.
4.1.3 taste and taste
When the sticky paste state, with a clear sour, astringent, spicy and sweet feeling on the palate and throat irritation. After swallowing or spitting, throat irritation still
It will persist for some time. When frozen, the early taste grainy, gradually disappeared, and the emergence of the state viscous paste the same taste.
4.1.4 Status
After thawing at room temperature or viscosity slurry was having liquidity. There should be no bubbles and impurities (such as wax shavings, etc.).
4.2 rating
According to the physical and chemical quality, Royal Jelly divided into superior products, and qualified for two levels.
4.3 Physical and Chemical Requirements
Product grades and physical and chemical requirements in Table 1.
Table 1 - Product grades and physical and chemical requirements
Index Top Qualified
Moisture /% ≤ 67.5 69.0
10- hydroxy-2-decanoic acid /% ≥ 1.8 1.4
Protein/11 ~ 16%
Total sugar (glucose) /% ≤ 15
Ash /% ≤ 1.5
Acidity (1mol/LNaOH)/(mL/100g) 30 ~ 53
Starch shall not be detected
4.4 Health and Safety Requirements
It should be consistent with national laws, regulations and government regulatory requirements, compliance with the relevant national standards of health and safety requirements.
4.5 Authenticity requirements
You can not add or remove any of the ingredients.
5 Test methods
Unless otherwise specified, all reagents were analytical method used reagents, water is distilled water.
5.1 Sample Preparation
Stainless steel rod, pipe or spoon as a sampler. The internal sample into the vial, stir evenly mixed, as the sample.
Each sample shall be not less than 20g.
After the sample should be tested immediately. If not timely test should be stored frozen at -18 ℃ refrigerator.
5.2 Water
5.2.1 Instruments
a) vacuum drying oven;
b) weighing bottle. high 25mm, diameter 35mm;
c) analytical balance. a sense of the amount of 0.0001g.
5.2.2 Test procedure
Take royal jelly samples of about 0.5g, put dried to constant weighing bottle, accurately weighed, smoothing, placed in a vacuum oven at a temperature
75 ℃, pressure -0.095MPa ~ -0.10MPa (-730mmHg ~ -760mmHg) Remove the weighing bottle and dried under 4h, set dry
Dryer, cooled 30min after weighing, repeated drying up twice before and after the quality difference is not more than 2mg, is constant.
5.2.3 Calculation
Royal Jelly moisture content according to equation (1).
100 (1)
Where.
X1 --- royal jelly moisture content,%;
5.2.4 parallel test relative deviation
Parallel test relative deviation should not exceed 0.8%.
5.3 10- hydroxy-2-decanoic acid
5.3.1 Reagents
This test water re-distilled water.
a) methanol. pure UV detection wavelength or transmittance of more than 30% of analytical grade.
b) ethanol. pure class distinctions.
c) Internal standard. methyl paraben, content 99.0%.
d) 10-HDA standard. 99.0% or more. Dried under reduced pressure within 24h prior to use in concentrated sulfuric acid was placed in a decompression drier.
e) 10-HDA standard solution. take dried after 10-HDA standard about 25mg, accurately weighed, add ethanol dissolved and transferred
25mL volumetric flask, diluted with ethanol to the mark. This solution per ml 10-HDA about 1mg.
f) Internal standard solution. take dried over methylparaben about 650mg, accurately weighed, add ethanol dissolved and transferred
1000mL volumetric flask, diluted with ethanol to the mark. The solution containing the internal standard per ml to about 0.65mg.
g) HCl (Ba = 0.03mol/L). amount of 0.1mol/L hydrochloric acid, 100mL, 200mL bidistilled water was added.
h) Mobile phase (CH3OH + 0.03mol/LHCl + H2O) = 55 + 10 + 35.
5.3.2 Instruments
a) high-performance liquid chromatograph. with UV detector, recorder or microprocessor;
b) Column. 4.6mm × 250mm stainless steel column filled with amorphous silica C18 bonded phase, 5μm or 10μm;
c) ultrasonic cleaning;
d) Vortex unit;
e) Analytical balance. a sense of the amount of 0.0001g.
5.3.3 Test procedure
5.3.3.1 Sample Processing
Samples were thawed to room temperature and stir with a glass rod, take about 0.5g, has weighed into the 50mL volumetric flask, accurately weighed,
0.03mol/L hydrochloric acid 1mL and water 2mL, SRE Vortex is mixed to dissolve the sample, add ethanol 30mL, while adding side lightly
Shake, then precision internal standard solution 10mL, and diluted with ethanol to the mark, shake, immediately set an ultrasonic bath ultrasonic 15min, or
SRE Vortex oscillation is 15min, was taken out and after 10min at 3000r/min centrifugation. If they can not be measured in time, should be placed in
Refrigerator cold test.
5.3.3.2 chromatographic conditions
Measurement wavelength. 210nm; Column temperature. 35 ℃; mobile phase flow rate. 1mL/min.
5.3.3.3 Determination of the correction factor
Precision drawing 10-HDA standard solution 0.5,1,2,3,4,5mL to 10mL volumetric flask. Precision internal standard solution 2mL, with
Ethanol diluted to the mark. Pipette solution 2μL, into the chromatograph, calculated using the peak area ratio should be linear, find school
Positive factor F.
5.3.3.4 sample measurement
Draw sample solution 4μL, into the chromatograph, press the "internal standard method" quantitative.
5.3.4 Calculation
Royal Jelly 10- hydroxy-2-decanoic acid content according to formula (2).
100 (2)
Where.
X2 --- royal jelly 10- hydroxy-2-decanoic acid content,%;
F --- the correction factor;
As --- internal standard peak in the sample area;
5.3.5 parallel test relative deviation
Parallel test the relative deviation of not more than 2.0%.
5.4 Protein
5.4.1 Reagents
a) concentrated sulfuric acid (ω = 95% ~ 98%);
b) copper sulfate and potassium sulfate mixed reagent. Weigh copper sulfate 1g, potassium sulfate 10g, set mortar mixed, fine spare;
c) mixed indicator. amount of ethanol solution of methyl red (ρ = 1g/L) 2 parts, bromocresol green ethanol solution (ρ = 2g/L) 3 parts, and mix;
d) boric acid absorption solution (ρ = 20g/L). Weigh boric acid 2.0g, placed in 100mL stoppered graduated cylinder, add ethanol 20mL, and add distilled
Diluted with water to the mark, shake to make boric acid dissolved spare;
e) sodium hydroxide solution (ρ = 400g/L). Weigh sodium hydroxide 40g, add distilled water to 100mL;
f) sulfuric acid. amount of concentrated sulfuric acid 5.7mL, add distilled water to 100mL;
g) hydrochloric acid standard solution (0.1mol/L). prepared according to GB/T 601 and calibration. Before using the exact diluted 10-fold.
5.4.2 Instruments
a) Kjeldahl method digestive apparatus, 50mL Kjeldahl flask (such as using far infrared furnace is equipped with 50mL Digestion Digestion tube plus gooseneck
funnel);
b) 10mL Acid burette;
c) analytical balance. a sense of the amount of 0.0001g;
d) semi-micro distillation apparatus Act (see Appendix A).
5.4.3 Test procedure
Cleaning 5.4.3.1 distillation unit
Connecting the distillation apparatus, A flask add appropriate amount of distilled water and a few drops of methyl red indicator solution, add dilute sulfuric acid into the acid, add a few glass beads or zeolite
Tablets, add distilled water from the funnel D about 50mL, G closed folder, open the condensed water, boil A bottle of distilled water. When the tip of the cold vapor from the condenser
When the condensate out, remove the source of fire, clip off H, C bottle of distilled water to make anti rushed B bottle. G to open the folder, release B bottle of distilled water, off B
Bottles and G folders. The condenser tube tip immersed in about 50mL of distilled water, distilled water so that the tip of the recoil to C condenser from the bottle, and then rushed to the B bottle, such as
The law to put distilled water. The instrument thus washed 2 or 3 times.
5.4.3.2 digest
Take a sample of approximately 1g royal jelly has been called on a given set of filter paper, accurately weighed after wrap, placed in Kjeldahl flask or digestion tube. Copper sulfate was added
Reagent is mixed with potassium 2g, then concentrated sulfuric acid was added slowly along the sidewall 10mL, thoroughly mixed, put in a small bottle funnel, the flask into a 45 ° oblique
Is set to start at a lower temperature is gradually heated, the solution was maintained at a temperature below the boiling point, after intumescent stop, and gradually increase the power, to be digested solution
Boiling, but not to remain in this state solution overflows into the clarity of the solution until the green heating was continued for 30min, transferred to a cooling capacity of 100mL
Flask, diluted with distilled water to the mark, shake spare.
5.4.3.3 Distillation
Amount of 20g/L boric acid solution 10mL, set 100mL conical flask, add 5 drops of mixed indicator, the tip of the condenser is immersed in the liquid under
Later, precision drawing above the digestion solution 5mL, transferred via D funnel reaction tube, then add 400g/L sodium hydroxide solution 10mL,
D funnel with a small amount of distilled water several times, clip off G, D addend ml of distilled water in the funnel to a closed pipeline. Heating A bottle (bottle steamed
Distilled water should be kept acidic solution of sulfuric acid), steam distillation, from the time of boric acid solution starting from wine red to blue-green from the distillation continued
After 10min, the tip of the condenser raised surface, so that the steam continue flushing 1min, with a small amount of distilled water rinse tip, distillation was stopped.
5.4.3.4 titration
The absorption liquid with 0.01mol/L hydrochloric acid standard solution titration to the blue-green to gray-purple as the end point.
5.4.4 Calculation
Royal jelly protein content according to equation (3) Calculated.
X3 =
(Vp Vp 1- 0) × 1 × 0.014 Ba
× 6.25 × 100 (3)
Where.
X3 --- royal jelly protein content, expressed in mass fraction,%;
Vp 1 --- Sample Titration 0.01mol/L of hydrochloric acid standard solution consumed volume in milliliters (mL of);
V0 --- titration blank 0.01mol/L hydrochloric acid standard solution consumed volume in milliliters (mL);
1 --- Ba concentration of hydrochloric acid standard solution, unit mole per liter (mol/L);
0.014 mmol --- nitrogen mass in grams (g);
6.25 --- protein nitrogen conversion factor.
Parallel test of the relative deviation 5.4.5
Parallel test relative deviation should not exceed 3.0%.
5.5 Total sugar
5.5.1 Reagents
a) glucose standard solution. precision learn dried to constant weight of 98 ℃ ~ 100 ℃ pure glucose (specific rotation + 52.5 ° ~
+ 53 °) 1.000g, add distilled water after hydrochloric acid was added to dissolve 5mL, and diluted with distilled water to 1000mL, this solution per milliliter
Equivalent to 1mg glucose.
b) Tongjia alkaline tartrate solution. Weigh copper sulfate (CuSO4 · 5H2O) 15g and methylene blue 0.05g, add distilled water and dilute
Diluted to 1000mL, stored in Mesa bottle.
c) alkaline copper tartrate solution B. Weigh sodium hydroxide and sodium potassium tartrate 50g 75g, add distilled water, was added potassium ferrocyanide
4g, wait until completely dissolved, diluted with distilled water to 1000mL, stored in Mesa polyethylene plastic bottle.
Calibration alkaline copper tartrate solution. precision drawing Tong Jia alkaline tartrate solution and Solution B each 5mL, placed in 150mL flasks
, Add distilled water 10mL, plus glucose standard solution from burette about 9mL, in 2min controlled heating to boiling, while boiling every 2s
Drop speed 71/92 glucose standard solution until the solution just faded blue as the end point, recording the consumption of glucose standard solution
Total volume, three simultaneous parallel operation, the mean value is calculated (liquid A, liquid B each 5mL) with an alkaline copper tartrate solution per 10mL
When the quality of glucose (mg).
d) zinc acetate solution (ρ = 219g/L). Weigh zinc acetate 21.9g, ice acetic acid 3mL, add distilled water and dilute to
100mL.
e) a solution of potassium ferrocyanide (ρ = 106g/L).
f) concentrated hydrochloric acid (ω = 36% ~ 38%).
g) HCl (Ba = 6mol/L). amount of hydrochloric acid 50mL, diluted with distilled water to 100mL.
h) sodium hydroxide solution (ρ = 200g/L).
i) Methyl red indicator solution (ρ = 1g/L, ethanol).
5.5.2 Instruments
a) electric heated water bath. Temperature fluctuation ± 1 ℃;
b) analytical balance, sense of volume 0.0001g, or electronic balance, a sense of the amount of 0.001g.
5.5.3 Test procedure
5.5.3.1 Sample Processing
Royal jelly is added slowly accurately weighed sample of about 4g, placed in 100mL flask, add distilled water 50mL, shaking after sample dissolution
Zinc acetate solution and a solution of potassium ferrocyanide 5mL, add distilled water to the mark. After standing 30min dry filter paper,
Filtrate was discarded early a few ml of the filtrate set aside.
Precision drawing preceding filtrate 50mL, 100mL flask placed, and hydrochloric acid (Ba = 6mol/L) 10mL, shake, put electric
Constant temperature water bath at 68 ℃ ~ 70 ℃ hydrolysis 10min, water cooled to room temperature, add 2 drops of methyl red indicator solution, shake, hydroxide
Sodium solution (ρ = 200g/L) and to the solution was yellow, add distilled water to the mark, shake, as the sample solution spare.
5.5.3.2 titrated sample solution
Tong Jia precision drawing alkaline tartrate solution and Solution B each 5mL, placed in 150mL conical flask, add distilled water 10mL, control
2min heated to boiling, to slow down after the speed, dropping the sample solution from the buret and keep the solution boiling until the solution color lighter
When every 2s drop speed titration until the blue just fade as the end point, the volume of consumption recorded in the sample solution.
5.5.4 Calculation
Royal Jelly total sugar content by the formula (4) Calculated.
X4 = T
2 × 1000
× 100 (4)
Where.
X4 --- royal jelly total sugar (glucose) content, expressed in mass fraction,%;
T --- alkaline copper tartrate solution titer, 10mL alkaline copper tartrate solution (solution A, solution B each 5mL) equivalent glucose
Mass, in milligrams (mg);
Vp 2 volumes of the sample solution consumed when --- titration, in milliliters (mL).
5.5.5 parallel test relative deviation
Parallel test relative deviation should not exceed 3.0%.
5.6 Ash
5.6.1 Reagents
Concentrated sulfuric acid (ω = 95% ~ 98%).
5.6.2 Instruments
a) analytical balance. a sense of the amount of ± 0.0001g;
b) quartz or porcelain crucible. 30mL;
c) dryers. built-in desiccant silica gel;
d) high-temperature furnace.
5.6.3 Test procedure
5.6.3.1 according to GB/T 5009.4-2003 4.1 execution.
5.6.3.2 jelly precisely weighed sample of about 1.5g, burning has been placed in a crucible to constant, low heat before heating the sample to fully carbonized
Smoking. Cooling to room temperature, concentrated sulfuric acid was added 0.5mL ~ 1mL, wetting the sample. Low temperature heating divisible sulfuric acid vapor. Set high-temperature furnace,
Firing at 700 ℃ ~ 800 ℃ to no carbon particles, namely ash completely. After the temperature dropped to below 200 ℃ removed, placed in the dryer to cool to room
Temperature and weighed. Repeat twice before and after burning to weigh no more than 0.3g difference is constant.
5.6.4 Calculation
Royal Jelly ash content according to equation (5) Calculated.
100 (5)
Where.
X5 --- royal jelly ash content, expressed in mass fraction,%;
5.6.5 parallel test relative deviation
Parallel test the relative deviation of not more than 2.0%.
5.7 Acidity
5.7.1 Reagents
Sodium hydroxide solution (Ba = 0.1mol/L). according to GB/T 601 standard preparation and calibration.
5.7.2 Instruments
a) pH meter. pH value accuracy of 0.1;
b) Buret. 10mL;
c) analytical balance. a sense of volume and a sense of volume ± 0.0001g ± 0.001g.
5.7.3 Test procedure
Weigh royal jelly samples 1.00g, placed in 100mL beaker, add freshly boiled and cooled distilled water 75mL, with sodium hydroxide
Standard solution (Ba = 0.1mol/L) titrated to pH meter indicates pH8.3 as the end point.
5.7.4 Calculation
Concentration titration value in ml of sodium hydroxide standard solution consumed (mol/L) is multiplied, multiplied by 100, is the acidity of the sample.
5.7.5 parallel test relative deviation
Parallel test the relative deviation of not more than 5%.
5.8 starch
5.8.1 Reagents
Iodine solution (ρ = 13g/L). Weigh iodine 1.3g, potassium iodide 3.6g, placed in 200mL beaker, add distilled water 30mL, plus concentrated hydrochloric
After a drop of acid dissolution add distilled water to 100mL, stir well, put a brown bottle, Mesa spare.
5.8.2 Test procedure
After the royal jelly samples weighed approximately 0.2g, a 50mL beaker, add distilled water 10mL, stir, heated to boiling, cooled to room temperature
Was added iodine (ρ = 13g/L) a few drops can not be blue.
6 packaging, labeling, storage, transport
6.1 Packaging
Containers should comply with health and safety requirements, packaging tight and firm.
6.2 mark
Packaging should be marked on the product name, origin, purchasing units, inspector name, date of acquisition, net weight/gross weight and tare.
When used as a pre-packaged food, its label should be consistent with GB 7718 requirements.
Transport packaging should be marked with product name, quantity and transportation icon logo.
6.3 Storage
Storage temperature should be below -18 ℃.
From different areas at different times of the production of royal jelly to be stored separately (bottling, packing).
Shall not smell, toxic, corrosive and polluting items may put the same stock.
6.4 Transport
Cold chain should not be with the smell, toxic, corrosive and potentially polluting materials loaded with mixed transport.
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