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(Zanthoxylum bungeanum and Zanthoxylum bungeanum processed products-Determination of total content of prickly amide)
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Basic data | Standard ID | GH/T 1291-2020 (GH/T1291-2020) | | Description (Translated English) | (Zanthoxylum bungeanum and Zanthoxylum bungeanum processed products-Determination of total content of prickly amide) | | 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 | GHT1291-2020: (Zanthoxylum bungeanum and Zanthoxylum bungeanum processed products-Determination of total content of prickly amide)
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Prickly ash and its processed products-Determination of total fagaramide-High performance liquid chromatography
ICS 67.220.10
B 36
GH
Industry Standards for Supply and Marketing Cooperation of the People's Republic of China
Determination of the total content of prickly amide in Zanthoxylum bungeanum and its processed products
High performance liquid chromatography
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., China Chamber of Commerce of Foodstuffs, Native Produce and Animal Husbandry Import and Export Association.
The main drafters of this standard. Liu Yingjie, Liu Qiang, Yang Qingshan, Zhang Hui, Zhao Botao, Liu Jihua, Wu Yaming, Cheng Yuanxin, Wang Yinliang,
Wang Yangai, Huang Xiaode, Wu Yaojun, Su Hai, Li Yi.
Zanthoxylum bungeanum and its processed products—Determination of total prickly amide content. High performance liquid chromatography
1 Scope
This standard specifies the high performance liquid chromatography method for the determination of the total content of prickly amides in Zanthoxylum bungeanum and its processed products.
This standard applies to the analysis and inspection of Zanthoxylum bungeanum and its processed products.
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 6682 Analytical laboratory water specifications and test methods
GB/T 12729.2 Sampling method for spices and condiments
GB/T 12729.3 Preparation of powder samples for analysis of spices and condiments
3 Terms and definitions
3.1
Prickly ash products
Zanthoxylum bungeanum is a product produced by processes such as crushing and extraction. Mainly including prickly ash powder, prickly ash oleoresin, prickly ash oil and other processing with prickly ash as raw materials
The product.
3.2
Fagaramide
Zanthoxylum bungeanum is the main ingredient of numb flavor, containing hydroxy-α-sanshool, hydroxy-β-sanshool, hydroxy-γ-sanshool and hydroxy-ε-sanshool, etc.
Kind of amide ingredients.
4 Principle
Xanthoxyamide substances mainly include hydroxy-α-sanshool, hydroxy-β-sanshool, hydroxy-γ-sanshool and hydroxy-ε-sanshool, etc.
Amide components, the prickly amide components in the sample are extracted by methanol, and then separated by a C18 column, using a high-performance liquid phase equipped with a UV detector
Chromatography was measured at 270 nm, with hydroxyl-α-sanshool as a reference substance, and the total amount of prickly amide in the sample was measured by the peak area external standard method.
Line determination.
5 Reagent materials and equipment
5.1 Reagent materials
5.1.1 Acetonitrile. chromatographically pure.
5.1.2 Methanol. chromatographically pure.
5.1.3 Glacial acetic acid. analytically pure.
5.1.4 Hydroxy-α-sanshool, CAS number. 83883-10-7, purity ≥95%.
5.1.5 Microporous filter membrane, organic phase filter membrane with a pore size of 0.22 μm.
5.2 Equipment
5.2.1 High performance liquid chromatograph equipped with ultraviolet detector.
5.2.2 Analytical balance, with a sensitivity of 0.0001 g and 0.0001 g.
5.2.3 Water bath.
5.2.4 Ultrasonic cleaner, ultrasonic power 240 W.
5.2.5 High-speed pulverizer, rotating speed ≥10 000 rpm.
6 Sample preparation
6.1 Standard solution preparation
Take 10 mg of hydroxy-α-sanshool reference substance (accurate to 0.1 mg), place it in a beaker, dissolve it with chromatography grade methanol, and dilute to 10 mL;
Dilute with chromatographic grade methanol to prepare reference substances with concentrations of 5 μg/mL, 10 μg/mL, 20 μg/mL, 30 μg/mL, 40 μg/mL, and 50 μg/mL
Working solution, to be tested.
6.2 Preparation of sample solution
6.2.1 Dried pepper
Take 100 g of the well-mixed peppercorns, pulverize with a high-speed grinder, pass through a 20-mesh sieve, and mix. Weigh 1 g (accurate to 0.0001 g) and crush
Place the mixed sample in a flask with a stopper, add 50 mL of methanol, extract with ultrasound for 0.5 h, cool to room temperature, and transfer to a 100 mL flask.
Constant volume, transfer 10 mL of the supernatant to a 50 mL volumetric flask to constant volume, filter through 0.22 μm filter membrane, to be tested.
6.2.2 Fresh pepper
Take.200 g of freshly mixed fresh pepper seeds. After being crushed by the tissue crusher, weigh 5 g (accurate to 0.0001 g) of the sample after crushing and mixing
Place it in a flask with a stopper, add 50 mL of methanol, ultrasonically extract for 0.5 h, cool to room temperature, transfer to a 100 mL flask, dilute the volume of methanol, and remove.
10 mL of the clear solution was put in a 50 mL volumetric flask and passed through a 0.22 μm filter membrane for testing.
6.2.3 Pepper powder
Weigh 1 g (accurate to 0.0001 g) of the crushed and mixed sample and place it in a flask with a stopper, add 50 mL of methanol, ultrasonically extract for 0.5 h, and cool
To room temperature, transfer to a 100 mL volumetric flask, make methanol to a constant volume, filter through a 0.22 μm filter membrane, and wait for measurement.
6.2.4 Zanthoxylum oleoresin
Take the paste or solid oleoresin sample to dissolve in a 50 ℃ water bath and shake well. Precisely weigh 0.2 g (accurate to 0.0001 g) sample set
In a beaker, add 50 mL of methanol, ultrasonically extract for 0.5 h, cool to room temperature, transfer to a 100 mL flask, make constant volume of methanol, filter through 0.22 μm
Membrane filtration, to be tested.
6.2.5 Pepper oil
Shake the pepper oil, accurately weigh 0.2 g (accurate to 0.0001 g) into a flask with a stopper, add 50 mL of methanol, and extract with ultrasound for 0.5 h.
Cool to room temperature, transfer to a 100 mL volumetric flask, make constant volume with methanol, filter with 0.22 μm filter membrane, and wait for measurement.
7 Analysis and calculation
7.1 Chromatographic conditions
--Chromatographic column. C18 reverse phase column, 4.6×150 mm, 5.0 μm, or equivalent.
--Mobile phase. acetonitrile.1% glacial acetic acid aqueous solution (40.60, V/V).
--Flow rate. 1.5 mL/min.
--Column temperature. 40 ℃.
--Sampling volume. 20 μL.
--Detection wavelength. 270 nm.
7.2 Drawing of standard curve
Measure the working solution (6.1) of the series of reference substances according to the measurement conditions (7.1), and take the peak area of the chromatographic peak as the ordinate, corresponding to the
Draw a standard curve with concentration as the abscissa of the solution.
7.3 Sample determination
Measure the sample solution (6.2) according to the determination condition (7.1), and qualitatively determine the prickly amide in the sample solution according to the retention time and spectrum. by
The total area of the characteristic peaks of the prickly amides in the sample liquid, the corresponding concentration of hydroxy-α-sanshool from the standard curve, the response of the sample liquid
The value should be within the linear range measured by the instrument, and the test sample solution that exceeds the linear range should be diluted with methanol and measured.
7.4 Calculation of results
The sum of the area of the 4 kinds of prickly amides was used as the area of prickly amide in the test product. The total content of Xanthamide in the test product is based on hydroxyl
Base-α-sanshool is calculated according to formula (1).
X--The total content of Xanthoamide in the test product, in milligrams per gram (mg/g);
C--The mass concentration corresponding to the peak area of Xanthoxylin in the test solution, in micrograms per milliliter (μg/mL);
V--The constant volume of the working solution of the test sample, in milliliters (mL);
K--The dilution factor of the working solution of the test sample;
m--The weight of the sample to be tested, in grams (g);
Take the arithmetic mean of the two measurement values with the absolute difference obtained under repeatability conditions not greater than 5% of the arithmetic mean as the measurement result
If the result is 2 decimal places.
AA
Appendix A
(Informative appendix)
Typical high performance liquid chromatogram
A.1 A typical high performance liquid chromatogram of hydroxy-α-sanshool is shown in Figure A.1.
A.2 A typical high performance liquid chromatogram of the sample solution is shown in Figure A.2.
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