NY/T 939-2016 PDF English
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Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
NY/T 939-2016 | English | 85 |
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Identification of Reconstituted Milk in Pasteurized and UHT Milk
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NY/T 939-2005 | English | 70 |
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Identification of reconstituted milk in pasteurized and UHT milk
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NY/T 939-2016: Identification of Reconstituted Milk in Pasteurized and UHT Milk---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/NYT939-2016
AGRICULTURE INDUSTRY STANDARD
ICS 67.050
X 04
Replacing NY/T 939-2005
Identification of Reconstituted
Milk in Pasteurized and UHT Milk
Issued on. MARCH 23, 2016
Implemented on. APRIL 01, 2016
Issued by. Ministry of Agriculture of PRC
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative References... 4
3 Terms and Definitions... 4
4 Test Methods... 5
5 Identification of Reconstituted Milk... 16
Appendix A (Informative) Furosine Liquid Chromatogram... 18
Foreword
This Standard was drafted as per the rules specified in GB/T 1.1-2009.
Compared with NY/T 939-2005, this Standard has the major changes as follows.
--- Modify the index value for the identification of reconstituted milk in the
pasteurized milk;
--- Modify the index value for the identification of reconstituted milk in the UHT milk;
--- Modify the pre-treatment method for furosine determination;
--- Add the UPLC determination of furosine;
--- Modify the determination of lactulose.
This Standard was proposed by the Department of Animal Husbandry, Ministry of
Agriculture.
This Standard shall be under the jurisdiction of National Technical Committee for
Standardizations of Animal Husbandry (SAC/TC 274).
Drafting organizations of this Standard. Institute of Animal Science of CAAS;
Laboratory of Quality & Safety Risk Assessment for Diary Products (Beijing), Ministry
of Agriculture; and Ministry of Agriculture – Milk and Dairy Product Inspection Center
(Beijing).
Chief drafting staffs of this Standard. Zheng Nan, Wen Fang, Wang Jiaqi, Li Songli,
Zhang Yangdong, Zhao Shengguo, Li Ming, Yang Jinhui, Chen Chongchong, Wang
Xiaoqing, Chen Meixia, Wang Hui, Lan Xinyi, Hang Mengmeng, Bo Dengpan, Wei
Hongyang, Li Shucong, Yu Jianguo, and Zhou Lingyun.
Identification of Reconstituted
Milk in Pasteurized and UHT Milk
1 Scope
This Standard specifies the identification method of reconstituted milk in pasteurized
and UHT milk.
This Standard is applicable to the pasteurized and UHT milk.
2 Normative References
The following documents are essential to the application of this document. For the
dated documents, only the versions with the dates indicated are applicable to this
document; for the undated documents, only the latest version (including all the
amendments) are applicable to this document.
GB 5009.5 Determination of Protein in Foods
GB/T 6682 Water for Laboratory Use – Specifications
GB/T 10111 Generation of Random Numbers and Procedures Applied to Sampling
Inspection for Product Quality
3 Terms and Definitions
For the purposes of this document, the following terms and definitions apply.
3.1 Raw milk
The normal milk extruded from the breasts of the healthy dairy animals, it meets the
relevant national requirements and has no ingredient changes.
3.2 Reconstituted milk
The milk obtained by mixing a dried or concentrated dairy product with water in
proportion.
3.3 Heat treatment
The operation that uses heating technology with strength no less than pasteurization,
inhibiting the growth of the microorganisms and killing the microorganisms; while
controlling the physicochemical properties of the heated objects within the only limited
changes.
3.4 Pasteurization
The processing method used to effectively kill pathogenic microorganisms, namely, the
treatment method to keep at a low temperature for a long time (maintain for 30min at
63°C~65°C) or to keep at a high temperature for a short time (maintain for 15s at
72°C~76°C; or maintain for 10s~15s at 80°C~85°C).
3.5 Pasteurized milk
The liquid product with raw milk as the raw material, obtained by pasteurization
process, with the lactulose content less than 100mg/L.
3.6 Ultra high-temperature, UHT
The processing method for effectively killing microorganisms and inhibiting heat-
resistant spores; namely, heating to at least 132°C in a continuous flow state, and
maintaining a very short time of heat treatment.
4 Test Methods
4.1 Determination of furosine content
4.1.1 Principle
Hydrolyze the specimen by hydrochloric acid, then determine its protein content; after
diluting, the hydrolysate shall be analyzed by high performance liquid chromatography
(HPLC) or ultra-high-performance liquid chromatography (UPLC) under ultraviolet
(wavelength 280nm) detector and quantify by external standard method.
4.1.2 Reagents and materials
Unless otherwise specified, all reagents used in this method shall be analytical
reagents; and the water shall be Class-I water in the laboratory specified in GB/T 6682.
4.1.2.10 Furosine standard stock solution (500.0mg/L). convert the furosine standard
substance as per the Net Peptide Content provided by the standard substance
certificate; then use 3mol/L hydrochloric acid solution to formulate into a standard stock
solution. It can be stored for 24 months at -20°C.
4.1.2.12 Aqueous phase membrane. 0.22µm.
4.1.3 Instruments
4.1.3.1 High Performance Liquid Chromatograph. equipped with a UV detector or
diode array detector.
4.1.3.2 Ultra-High-Performance Liquid Chromatograph. equipped with a UV detector
or diode array detector.
4.1.3.3 Drying oven. (110±2) °C
4.1.3.4 Sealed heat-resistant test tube. volume of 20mL.
4.1.3.5 Balance. the sensitivity of 0.01mg, 1mg.
4.1.3.6 Kjeldahl apparatus.
4.1.6 Result calculation
4.1.6.1 Furosine content in the specimen
The furosine is calculated by mass fraction F; the value of which is expressed in
mg/100g protein; and calculated as per Formula (1).
4.1.6.3 Furosine content at the sterilization of UHT milk
At the end of sterilization of UHT milk, the furosine content shall be calculated by FT;
the value of which shall be expressed by mg/100 protein; and calculated as per
Formula (3).
4.2 Determination of lactulose content
4.2.1 Principle
The sample is hydrolyzed by β – D – galactosidase to produce galactose and fructose;
the lactulose content is calculated by the enzymatic determination of the amount of
fructose.
4.2.2.30 Glucose oxidase (GOD) suspension (20mg/mL). use sterilized water to
prepare the glucose oxidase with activity of 200 IU/mg into suspension with
concentration of 20mg/mL. It shall be prepared for current use.
4.2.2.31 Catalase suspension (20mg/mL). use sterilized water to prepare the catalase
with activity of 65000 IU/mg into suspension with concentration of 20mg/mL. It shall be
stored at 4°C; shake it before use to make it uniform.
4.2.3 Apparatus
4.3.3.1 Constant temperature incubator. (40±2) °C, (50±2) °C.
4.3.3.2 Spectrophotometer. 340nm.
4.2.4 Sampling
The same as 4.1.4.
4.2.5 Analytical procedures
4.3 Calculation of ratio between lactulose and furosine
The calculation result shall be retained two digits after the decimal point.
5 Identification of Reconstituted Milk
5.1 Pasteurized milk
When L< 100.0mg/L, it shall be judged as follows.
Appendix A
(Informative)
Furosine Liquid Chromatogram
A.1 Chromatogram of high-performance liquid chromatography (HPCL)
See Figures A.1 and A.2.
NY/T 939-2016
AGRICULTURE INDUSTRY STANDARD
ICS 67.050
X 04
Replacing NY/T 939-2005
Identification of Reconstituted
Milk in Pasteurized and UHT Milk
Issued on. MARCH 23, 2016
Implemented on. APRIL 01, 2016
Issued by. Ministry of Agriculture of PRC
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative References... 4
3 Terms and Definitions... 4
4 Test Methods... 5
5 Identification of Reconstituted Milk... 16
Appendix A (Informative) Furosine Liquid Chromatogram... 18
Foreword
This Standard was drafted as per the rules specified in GB/T 1.1-2009.
Compared with NY/T 939-2005, this Standard has the major changes as follows.
--- Modify the index value for the identification of reconstituted milk in the
pasteurized milk;
--- Modify the index value for the identification of reconstituted milk in the UHT milk;
--- Modify the pre-treatment method for furosine determination;
--- Add the UPLC determination of furosine;
--- Modify the determination of lactulose.
This Standard was proposed by the Department of Animal Husbandry, Ministry of
Agriculture.
This Standard shall be under the jurisdiction of National Technical Committee for
Standardizations of Animal Husbandry (SAC/TC 274).
Drafting organizations of this Standard. Institute of Animal Science of CAAS;
Laboratory of Quality & Safety Risk Assessment for Diary Products (Beijing), Ministry
of Agriculture; and Ministry of Agriculture – Milk and Dairy Product Inspection Center
(Beijing).
Chief drafting staffs of this Standard. Zheng Nan, Wen Fang, Wang Jiaqi, Li Songli,
Zhang Yangdong, Zhao Shengguo, Li Ming, Yang Jinhui, Chen Chongchong, Wang
Xiaoqing, Chen Meixia, Wang Hui, Lan Xinyi, Hang Mengmeng, Bo Dengpan, Wei
Hongyang, Li Shucong, Yu Jianguo, and Zhou Lingyun.
Identification of Reconstituted
Milk in Pasteurized and UHT Milk
1 Scope
This Standard specifies the identification method of reconstituted milk in pasteurized
and UHT milk.
This Standard is applicable to the pasteurized and UHT milk.
2 Normative References
The following documents are essential to the application of this document. For the
dated documents, only the versions with the dates indicated are applicable to this
document; for the undated documents, only the latest version (including all the
amendments) are applicable to this document.
GB 5009.5 Determination of Protein in Foods
GB/T 6682 Water for Laboratory Use – Specifications
GB/T 10111 Generation of Random Numbers and Procedures Applied to Sampling
Inspection for Product Quality
3 Terms and Definitions
For the purposes of this document, the following terms and definitions apply.
3.1 Raw milk
The normal milk extruded from the breasts of the healthy dairy animals, it meets the
relevant national requirements and has no ingredient changes.
3.2 Reconstituted milk
The milk obtained by mixing a dried or concentrated dairy product with water in
proportion.
3.3 Heat treatment
The operation that uses heating technology with strength no less than pasteurization,
inhibiting the growth of the microorganisms and killing the microorganisms; while
controlling the physicochemical properties of the heated objects within the only limited
changes.
3.4 Pasteurization
The processing method used to effectively kill pathogenic microorganisms, namely, the
treatment method to keep at a low temperature for a long time (maintain for 30min at
63°C~65°C) or to keep at a high temperature for a short time (maintain for 15s at
72°C~76°C; or maintain for 10s~15s at 80°C~85°C).
3.5 Pasteurized milk
The liquid product with raw milk as the raw material, obtained by pasteurization
process, with the lactulose content less than 100mg/L.
3.6 Ultra high-temperature, UHT
The processing method for effectively killing microorganisms and inhibiting heat-
resistant spores; namely, heating to at least 132°C in a continuous flow state, and
maintaining a very short time of heat treatment.
4 Test Methods
4.1 Determination of furosine content
4.1.1 Principle
Hydrolyze the specimen by hydrochloric acid, then determine its protein content; after
diluting, the hydrolysate shall be analyzed by high performance liquid chromatography
(HPLC) or ultra-high-performance liquid chromatography (UPLC) under ultraviolet
(wavelength 280nm) detector and quantify by external standard method.
4.1.2 Reagents and materials
Unless otherwise specified, all reagents used in this method shall be analytical
reagents; and the water shall be Class-I water in the laboratory specified in GB/T 6682.
4.1.2.10 Furosine standard stock solution (500.0mg/L). convert the furosine standard
substance as per the Net Peptide Content provided by the standard substance
certificate; then use 3mol/L hydrochloric acid solution to formulate into a standard stock
solution. It can be stored for 24 months at -20°C.
4.1.2.12 Aqueous phase membrane. 0.22µm.
4.1.3 Instruments
4.1.3.1 High Performance Liquid Chromatograph. equipped with a UV detector or
diode array detector.
4.1.3.2 Ultra-High-Performance Liquid Chromatograph. equipped with a UV detector
or diode array detector.
4.1.3.3 Drying oven. (110±2) °C
4.1.3.4 Sealed heat-resistant test tube. volume of 20mL.
4.1.3.5 Balance. the sensitivity of 0.01mg, 1mg.
4.1.3.6 Kjeldahl apparatus.
4.1.6 Result calculation
4.1.6.1 Furosine content in the specimen
The furosine is calculated by mass fraction F; the value of which is expressed in
mg/100g protein; and calculated as per Formula (1).
4.1.6.3 Furosine content at the sterilization of UHT milk
At the end of sterilization of UHT milk, the furosine content shall be calculated by FT;
the value of which shall be expressed by mg/100 protein; and calculated as per
Formula (3).
4.2 Determination of lactulose content
4.2.1 Principle
The sample is hydrolyzed by β – D – galactosidase to produce galactose and fructose;
the lactulose content is calculated by the enzymatic determination of the amount of
fructose.
4.2.2.30 Glucose oxidase (GOD) suspension (20mg/mL). use sterilized water to
prepare the glucose oxidase with activity of 200 IU/mg into suspension with
concentration of 20mg/mL. It shall be prepared for current use.
4.2.2.31 Catalase suspension (20mg/mL). use sterilized water to prepare the catalase
with activity of 65000 IU/mg into suspension with concentration of 20mg/mL. It shall be
stored at 4°C; shake it before use to make it uniform.
4.2.3 Apparatus
4.3.3.1 Constant temperature incubator. (40±2) °C, (50±2) °C.
4.3.3.2 Spectrophotometer. 340nm.
4.2.4 Sampling
The same as 4.1.4.
4.2.5 Analytical procedures
4.3 Calculation of ratio between lactulose and furosine
The calculation result shall be retained two digits after the decimal point.
5 Identification of Reconstituted Milk
5.1 Pasteurized milk
When L< 100.0mg/L, it shall be judged as follows.
Appendix A
(Informative)
Furosine Liquid Chromatogram
A.1 Chromatogram of high-performance liquid chromatography (HPCL)
See Figures A.1 and A.2.
...... Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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