GB/T 39999-2021 in English
VALIDDetermination of 15 kinds of prohibited quinolone-type antibiotics in cosmetics including enrofloxacin—Liquid chromatography-tandem mass spectrometry
- Issued on:2021-04-30
- Implemented on:2021-11-01
- File Format:PDF
- Delivery:Via email within 1~3 business days
$214.00
《GB/T 39999-2021化妆品中恩诺沙星等15种禁用喹诺酮类抗生素的测定 液相色谱-串联质谱法》由TC257（全国香料香精化妆品标准化技术委员会）归口，TC257SC2（全国香料香精化妆品标准化技术委员会化妆品分会）执行，主管部门为中国轻工业联合会。
Introduction
Analysis of the core content of the standard
This standard establishes detection methods for 15 quinolone antibiotics that are explicitly prohibited by the "Technical Specifications for Safety of Cosmetics", including the key parameter settings of the liquid chromatography-triple quadrupole mass spectrometry and the sample pretreatment process.
Comparison of technical methods
| Technical elements | Characteristics of this method | Conventional HPLC method |
|---|---|---|
| Detection sensitivity | 0.15mg/kg detection limit | 1.0-5.0mg/kg |
| Analysis time | 10min/sample | 20-30min/sample |
| Anti-interference ability | MRM mode dual qualitative | Single wavelength detection |
Key operating points
Sample pretreatment: Double extraction with acidified acetonitrile (8mL×2 times) was used, and acetonitrile-saturated n-hexane was used for purification to effectively remove fat-soluble interferences.
Optimization of mass spectrometry conditions: In the ESI positive ion mode, the collision energy of each compound was controlled in the range of 15-55V, such as enrofloxacin (360.3→245.0) using a collision voltage of 55V.
Implementation Recommendations
- Laboratories need to regularly calibrate the mass axis of the triple quadrupole mass spectrometer
- Each batch of samples should be accompanied by blank controls and spike recovery experiments (control 80-110% range)
- For samples with high matrix interference, the proportion of n-hexane in the cleanup step can be adjusted
Standard Evolution Analysis
Compared with the 2015 version of the specification which only lists the banned substances, the innovations of this standard are:
- Establish a multi-component simultaneous detection scheme
- Introduce the expanded application space of the isotope internal standard method
- Clearly define the quantitative limit requirement of 0.50mg/kg
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