T/CIFST 007-2022 in English
VALIDDetermination of 2-fucosyllactose in foods— Ion chromatography method
- Issued on:2022-02-07
- Implemented on:-
- File Format:PDF
- Delivery:Via email within 1~3 business days
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本文件适用于婴幼儿配方食品、乳粉和特殊医学用途配方食品中2-岩藻糖基乳糖含量的测定。
Introduction
Technical background and significance of the standard
2'-fucosyllactose is an important functional oligosaccharide in breast milk. It has a significant prebiotic effect when added to infant formula. This standard fills the gap in the detection method of this ingredient in my country. It uses ion chromatograph combined with pulsed amperometric detection technology to solve the problem of insufficient sensitivity of traditional methods.
Core principles of the method
| Technical aspects | Key parameters | Innovation points |
|---|---|---|
| Sample pretreatment | Dual enzyme system (amyloglucosidase + β-galactosidase) | Enzymatic hydrolysis at 60℃ for 2 hours, conversion rate>95% |
| Chromatographic separation | Carbopac PA1 analytical column | Tri-gradient mobile phase (water/NaOH/sodium acetate) |
| Detection system | Four-potential pulse amperometric detection | Gold electrode working potential +0.1V～+0.3V |
Key Operation Points
Enzymatic Condition Control: It is necessary to ensure that the activity of amylotransferase in the enzyme mixture is ≥2.8U/0.2g sample, and the activity of β-galactosidase is ≥40U/0.2g sample. In actual application, it is found that when the pH deviates from 4.5±0.1, the enzyme activity will decrease by 30-50%.
Chromatographic System Maintenance: It is recommended to replace the pre-column after every 200 injections, and the mobile phase needs to be continuously protected by high-purity nitrogen to prevent carbonate precipitation.
Method Performance Verification
| Sample Type | Limit of Detection (LOD) | Limit of Quantitation (LOQ) | Spike Recovery |
|---|---|---|---|
| Solid Samples | 9mg/100g | 36mg/100g | 92-105% |
| Liquid Samples | 1mg/100g | 4mg/100g | 94-103% |
Implementation Recommendations
- Standard storage: After opening, the moisture content must be confirmed with a Karl Fischer titrator. Storage at -80°C can extend the shelf life to 8 months
- System suitability test: The intermediate concentration standard solution (25 mg/L) should be run before daily analysis, and the retention time drift should be <2.5%
- Quality control measures: It is recommended to insert a quality control sample every 10 samples and use the standard addition method to verify the matrix effect
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