SN/T 4675.16-2016 in English
VALIDDetermination of fumaric acid in wine for export-LC-MS/MS method
- Issued on:2016-12-12
- Implemented on:2017-07-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
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Introduction
Standard Overview
SN/T 4675.16-2016 specifies the liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of fumaric acid (CAS 110-17-8) in wine for export, with a detection limit of 2.5 mg/L. This standard applies to the export inspection of all types of wine products.
Key Technical Points
| Technical Steps | Parameter Requirements | Quality Control |
|---|---|---|
| Sample Pretreatment | 10 mL centrifuge tube, centrifugation at 8000 r/min for 5 minutes | 0.22μm PTFE membrane filtration |
| Chromatographic Conditions | T3 chromatographic column (2.1×50mm,1.8μm) | Mobile phase: 0.1% formic acid aqueous solution + acetonitrile |
| Mass Spectrometry Parameters | ESI negative ion mode, MRM monitoring | Characteristic ion pairs: m/z 115>71/27 |
Key points for standard implementation
Preparation of standard solutions
The standard requires the accurate preparation of gradient standard solutions (0.10-5.0μg/mL), including:
- Stock solution (1.0 mg/mL): weigh 50.7 mg of fumaric acid standard
- Intermediate solution (10μg/mL): take 0.5 mL of stock solution and dilute to 50 mL
- The working solution must be prepared and used immediately and stored at 4℃ for no more than 3 days
Method validation data
Standard validation shows:
- Spike recovery: 84.8%-106.5%
- Relative standard deviation (RSD): 2.02%-5.19%
- Linear range: 0.10-5.0μg/mL (r²≥0.999)
Technology Evolution Analysis
Compared with traditional HPLC methods, the LC-MS/MS technology used in this standard has the following advantages:
- Improved sensitivity: Detection limit reduced by more than 10 times
- Anti-interference ability: Elimination of matrix effects through MRM mode
- Analysis efficiency: Single run time <8 minutes
Application Recommendations
Laboratory Implementation Recommendations
- Mass spectrometer tuning requires optimization of collision energy (CE) to ensure that the characteristic ion abundance ratio meets the requirements of Appendix B
- A matrix-matched standard curve should be provided with each batch of samples.
- It is recommended to use the isotope internal standard method to improve quantitative accuracy.
Standard Update Tips
This standard references GB/T 1.1-2009 Guidelines for Standardization. Laboratories should note:
- The new version of GB/T 1.1-2020 to be released after 2020 has new requirements for the standard format.
- When the test results are close to the limit value, it is recommended to use ISO 11292:1995 for method comparison.

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