SN/T 5349-2021 in English
VALIDDetermination of siloxane compounds in silica gel heat-resisting material - GC-MS/MS method
- Issued on:2021-11-22
- Implemented on:2022-06-01
- File Format:PDF
- Delivery:Via email within 5 business days
$379.00
Introduction
Technical background and scope of application of the standard
This standard aims at the migration risk of 21 siloxane compounds in heat-resistant silicone materials and establishes a gas chromatography-tandem mass spectrometer detection method. It is applicable to the quality monitoring of silicone products in the fields of food contact materials, medical devices, etc.
Core technology innovation of the method
| Technical dimension | Traditional method | Improvement of this standard |
|---|---|---|
| Sample pretreatment | Grinding at room temperature leads to volatile loss | Liquid nitrogen freezing and crushing (-196℃) to maintain compound stability |
| Detection sensitivity | Single quadrupole mass spectrometry LOQ≥1mg/kg | MRM mode quantification limit of 0.1mg/kg |
| Anti-interference ability | Significant matrix effect | Using D5 isotope internal standard calibration |
Analysis of key operation points
Sample preparation case
In the detection of a medical silicone catheter, the sample was crushed to 150 mesh using a liquid nitrogen cryo-grinder, and then ultrasonically extracted with ethyl acetate at 40°C for 30 minutes, and the recovery rate was increased to 92-105%.
Mass spectrometry parameter optimization
For D4 (octamethylcyclotetrasiloxane), the parent ion m/z 281→265 daughter ion conversion was set, the collision energy was 25eV, and the signal-to-noise ratio was increased by 3 times.
Standard Implementation Recommendations
- Quality Control: Each batch of samples should be subjected to a blank spike experiment, and the recovery rate should be controlled at 80-120%
- Equipment Calibration: PFTBA standards should be used to calibrate the mass axis after daily startup
- Data Analysis: The ion abundance ratio deviation ≤ 20% is used as the positive judgment standard
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