SN/T 0535-2016 in English
VALIDDetermination of gossypol in feed for import and export
- Issued on:2016-08-23
- Implemented on:2017-03-01
- File Format:PDF
- Delivery:Via email within 5 business days
$301.00
本标准规定了饲料中棉酚的两种测定方法，高效液相色谱法和液相色谱-质谱/质谱法。
Introduction
Background of Standard Revision and Technological Evolution
This standard replaces the 1996 version of SN 0535. The main technical upgrades include: adding LC-MS/MS confirmation method, expanding matrix applicability to various feed types, and optimizing extraction process to improve recovery rate. It reflects the development of chromatographic detection technology in the past 20 years, especially the establishment of the authority of mass spectrometry technology in trace analysis.
Comparative analysis of method frameworks
| Dimensions | HPLC method | LC-MS/MS method |
|---|---|---|
| Detection limit | 10 mg/kg | 1 mg/kg |
| Quantitative principle | UV detection (238nm) | MRM mode (m/z 517.1→230.9) |
| Matrix effect | Interference peaks need to be considered | Eliminate interference by ion pairing |
| Precision (RSD) | 2.3-3.6% | 1.7-5.3% |
Analysis of key operation points
1. Pretreatment optimization
Use acetone-water (70:30) mixed extraction solution, soak in water for 1 hour to promote release, and then ultrasonic extraction. Compared with the original standard, the centrifuge tube material requirement (polypropylene) is added to avoid cottonphenol adsorption.
2. HPLC condition setting
- C18 column: 250mm×4.6mm, 5μm
- Mobile phase: methanol-0.1% phosphoric acid (88:12)
- Theoretical plate number at flow rate of 1.5mL/min>5000
Implementation suggestions and common problems
Case: Abnormal handling of cottonseed meal detection
The HPLC detection value of a batch of cottonseed meal was 92.04mg/kg, but LC-MS/MS confirmed it was 87.88mg/kg. The difference is due to the co-elution interference of HPLC. Suggestions:
- Optimize the gradient elution program (refer to Appendix A)
- When the HPLC result>50mg/kg, it must be verified by LC-MS/MS
Precautions for implementation of the standard
- The cottony phenol standard solution needs to be stored away from light (<4℃). The validity period verification shows that:
- The degradation rate is <5% when stored at -20℃ for 30 days
- The degradation rate is 12% at room temperature within 24 hours
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