GH/T 1291-2020 in English
VALIDPrickly ash and its processed products―Determination of total fagaramide―High performance liquid chromatography
- Issued on:2020-06-04
- Implemented on:2020-09-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
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本标准规定了花椒及花椒加工产品中花椒酰胺类物质总含量的高效液相色谱测定方法。
本标准适用于花椒及花椒加工产品的分析与检验。
Introduction
Technical background of the standard
This standard is under the jurisdiction of the National Technical Committee for Standardization of Spices and Flavors (SAC/TC 408) and is formulated to meet the testing requirements for pickle amides in pepper and its processed products. With the widespread application of pepper products in the condiment market, establishing a unified analytical method is of great significance to ensuring product quality.
Core Detection Principle
The four main sanshoamides were separated by high performance liquid chromatography (with UV detector) at a wavelength of 270 nm and a C18 reverse phase column. Hydroxy-α-sanshool was used as the reference substance and the external standard method was used to quantitatively analyze the following:
| Component Name | CAS No. | Relative Retention Time |
|---|---|---|
| Hydroxy-α-sanshool | 83883-10-7 | 1.00 (reference peak) |
| Hydroxy-β-sanshool | - | 1.12±0.05 |
| Hydroxy-γ-sanshool | - | 1.35±0.08 |
| Hydroxy-ε-sanshool | - | 1.62±0.10 |
Key Operation Points
Differences in Sample Pretreatment
Different pretreatment schemes were used for samples with different morphologies:
- Dried Zanthoxylum: needs to be crushed by a high-speed grinder (>10,000 rpm) and passed through a 20-mesh sieve
- Fresh Zanthoxylum: processed by a tissue crusher
- Zanthoxylum oleoresin: needs to be pre-dissolved in a 50℃ water bath
Optimization of chromatographic conditions
The mobile phase was acetonitrile-1% acetic acid aqueous solution (40:60, V/V), with a flow rate of 1.5 mL/min and a column temperature of 40°C. Under these conditions, the four amide components can be completely separated within 20 minutes.
Method Validation Data
The standard requires a linear range of 5-50 μg/mL and a correlation coefficient R²≥0.999. The absolute difference between the two determination results under repeatability conditions should not exceed 5% of the arithmetic mean.
Implementation Suggestions
- Reference material storage: Hydroxy-α-sanshool needs to be stored at -20℃ away from light
- System suitability test: Before each test, the separation degree must be confirmed to be ≥1.5
- Quality control measures: Each batch of samples should be tested in parallel for spiked recovery (85-105%)
Technology Evolution Comparison
| Detection indicators | This method | Traditional methods | Advantages |
|---|---|---|---|
| Detection limit | 0.1 mg/g | 0.5 mg/g | Sensitivity increased by 5 times |
| Analysis time | 20 min | 45 min | Efficiency increased by 125% |
| Component differentiation | 4 kinds of amides | Total amount determination | Strong component specificity |

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