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(Determination of volatile components of Zanthoxylum bungeanum Maxim. Gas chromatography-mass spectrometry)
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Basic data | Standard ID | GH/T 1294-2020 (GH/T1294-2020) | | Description (Translated English) | (Determination of volatile components of Zanthoxylum bungeanum Maxim. Gas chromatography-mass spectrometry) | | Sector / Industry | Supply and Marketing Cooperatives Industry Standard (Recommended) | | Classification of Chinese Standard | B36 | | Classification of International Standard | 67.220.10 | | Date of Issue | 2020-06-04 | | Date of Implementation | 2020-09-01 | | Regulation (derived from) | Industry Standard Information Service Platform (2020.07.22) | | Issuing agency(ies) | All-China Federation of Supply and Marketing Cooperatives | GHT1294-2020: (Determination of volatile components of Zanthoxylum bungeanum Maxim. Gas chromatography-mass spectrometry)
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Determination of volatile flavoured compounds in prickly ash-Gas chromatography-tadem mass spectrometry method
ICS 67.220.10
B 36
GH
Industry Standards for Supply and Marketing Cooperation of the People's Republic of China
Determination of Volatile Components in Zanthoxylum bungeanum Maxim. Gas Chromatography-Mass Spectrometry
2020-06-04 release
2020-09-01 Implementation
Released by China National Supply and Marketing Cooperatives
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
Appendix A of this standard is an informative appendix.
This standard was proposed by the All-China Federation of Supply and Marketing Cooperatives.
This standard is under the jurisdiction of the National Spice Standardization Technical Committee (SAC/TC 408).
Drafting organizations of this standard. All China Supply and Marketing Cooperatives Nanjing Institute of Comprehensive Utilization of Wild Plants, Shaanxi Weikang Food Technology Co., Ltd.
Co., Ltd., Chenguang Biological Technology Group Co., Ltd., Zhumadian Wangshouyi Shisanxiang Condiment Group Co., Ltd., Shandong Baijia Food
Co., Ltd., National Non-staple Food Quality Supervision and Inspection Center, China Chamber of Commerce for Foodstuffs, Native Produce and Livestock Import and Export, Seasoning Branch, Anhui Huace Testing Technology Co., Ltd.
Company, Pony Testing Group Shanghai Co., Ltd.
The main drafters of this standard. Liu Yingjie, Liu Qiang, Yang Qingshan, Zhang Hui, Zhao Botao, Liu Jihua, Wu Yaojun, Zhang Xiaofang, Wei Zhanjiao,
Wang Yinliang, Wang Yangai, Huang Xiaode, Chen Bin, Qian Hua, Su Hai, Li Yi, Xu Zhiqiang, Liu Jia, Jin Ze, Luo Liang, Zhang Yingjie, Shao Wei.
Determination of Volatile Components in Zanthoxylum bungeanum Maxim. Gas Chromatography-Mass Spectrometry
1 Scope
This standard specifies the determination of relative content of Zanthoxylum bungeanum volatile components in Zanthoxylum bungeanum, Zanthoxylum bungeanum powder and Zanthoxylum bungeanum oleoresin by gas chromatography-mass spectrometry
method.
This standard is applicable to the determination of the relative content of Zanthoxylum bungeanum volatile components in Zanthoxylum bungeanum, Zanthoxylum bungeanum powder and Zanthoxylum bungeanum oleoresin.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document.
For undated references, the latest version (including all amendments) applies to this document.
GB/T 12729.2 Sampling method for spices and condiments
GB/T 12729.3 Preparation of powder samples for analysis of spices and condiments
GB/T 30385-2013 Determination of volatile oil content of spices and condiments
3 Principle
After the volatile components in the sample are extracted by steam distillation, they are separated by a gas chromatographic column, and qualitatively detected by a mass spectrometer.
Chemical method was used to determine the relative content of volatile flavor components.
4 Reagents and instruments
4.1 Instrument
4.1.1 Gas chromatography-mass spectrometer. EI source.
4.1.2 High-speed grinder, rotating speed ≥10000 rpm.
4.1.3 Distiller (same as GB/T 30385-2013.6.1)
4.2 Reagents
4.2.1 Anhydrous sodium sulfate, analytically pure.
5 Sample processing
5.1 Pepper
After taking samples in accordance with GB/T 12729.2, remove the pepper seeds and impurities in the samples, and prepare powder samples in accordance with GB/T 12729.3
Product spare.
5.2 Pepper powder
After sampling according to GB/T 12729.2, mix evenly for later use.
6 Analysis steps
6.1 Extraction of volatile components
Sampling was carried out according to the sampling volume of 50.0 g of pepper and pepper powder and 10.0 g of pepper oleoresin, and added to the distiller, and adjusted the distillation rate
Keep distilling in the range of 2~3 mL/min for 4 h, stop heating and cooling for 10 min, collect volatile components, and add 2 g of anhydrous sulfur
Sodium is dehydrated and filtered through a 0.22 μm microporous membrane for testing.
6.2 Analysis conditions
6.2.1 Chromatographic conditions
a) Chromatographic column. HP-5MS (60 m×250 μm×0.1 μm) capillary gas chromatography column or equivalent column;
b) Carrier gas conditions. The carrier gas is high-purity helium with a flow rate of 1.0 mL/min;
c) Inlet temperature. 250℃, interface temperature 280℃;
d) Injection volume. 1 μL, split ratio 100.1;
e) Column thermostat heating program. the initial temperature is 60 ℃, keep for 2 min, increase the temperature to 135 ℃ at 2 ℃/min, keep for 10 min,
Then the temperature was increased to 240°C at 20°C/min and kept for 4 minutes.
6.2.2 Mass spectrometry conditions
a) Detection method. quality full scan mode, scan range 33～650 amu;
b) Ionization method. electron bombardment ionization source (EI source, electron energy 70 eV);
c) Ion source temperature. 230℃;
d) Transmission line temperature. 250℃;
e) Solvent delay. 3 min.
6.3 Sample determination
Inject the sample to be tested into a gas chromatography-mass spectrometer, set the mass spectrometer to automatically identify chromatographic peaks with a signal-to-noise ratio greater than 100, and use NIST
Qualitative database. The similarity of the mass spectrum is ≥80% of the chromatographic peak, and the relative content of each volatile flavor component is calculated according to the peak area normalization method
the amount.
7 Result calculation
The relative content Ci of a certain volatile wind component in the sample is calculated as the fraction of the peak area corresponding to the component to the sum of the peak areas of all components.
The value is expressed in% and calculated according to formula (1).
Ci-the peak area fraction of the volatile substance i in the sample, expressed as a percentage (%);
Asi-the peak area of the volatile component i in the sample;
∑Asi--the sum of the peak areas of the volatile flavor components in the sample.
The calculation result is expressed as the arithmetic mean of two independent determination results with absolute difference not greater than 5% of the arithmetic mean under repeatability conditions.
The result retains 2 digits after the decimal point.
AA
Appendix A
(Informative appendix)
Characteristic spectrum of typical volatile components of Zanthoxylum bungeanum
A.1 The total ion current chromatogram (TIC) of typical volatile components of red pepper is shown in Figure A.1, and the mass spectrometric identification results of typical volatile components of red pepper are shown in
Table A.1.
Figure A.1 Total ion chromatogram (TIC) of typical volatile components of red pepper
A.2 The total ion current chromatogram (TIC) of the typical volatile components of Green Zanthoxylum bungeanum is shown in Figure A.2, and the mass spectrum identification results of the typical volatile components of Green Zanthoxylum bungeanum are shown in
Table A.2.
Figure A.2 The total ion current chromatogram (TIC) of typical volatile components of green pepper
Table A.2 Mass spectrometric identification results of typical volatile components of Zanthoxylum bungeanum Maxim
Sequence number retention time
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