固相萃取-气相色谱-负化学离子源质谱法测定运动场所合成材料面层和稀释剂中的短链氯化石蜡

Determination of short-chain chloroparaffins in synthetic surfacing layers used in sports and diluents by solid-phase extraction coupled with gas chromatography-negative chemical ionization-mass spectrometry

建立了用于运动场所合成材料面层和稀释剂中短链氯化石蜡(SCCPs)总含量测定的固相萃取-气相色谱-负化学离子源质谱法(SPE-GC-NCI-MS)。对气相色谱和质谱的分析条件进行了优化;试样经超声提取、弗罗里硅土固相萃取小柱净化后,选择性离子监测模式(SIM)扫描,外标法定量。方法在0. 050 1~100. 17 mg/L的宽广范围内有良好的线性关系,线性相关系数R2为0. 999 5,方法检出限低至0. 50μg/g(即0. 000 050%),平均回收率为83. 2%~96. 3%,相对标准偏差为1. 56%~6. 02%。对10批次实际样品进行检测,含量在0. 016%~0. 55%范围内,检测结果满足欧盟对此类物质的限量要求。方法可用于运动场所合成材料面层和稀释剂中短链氯化石蜡的实际检测。

A new method was established to determine short-chain chloroparaffins （SCCPs） in synthetic surfacing layers used in sports and diluents by solid-phase extraction （SPE） coupled with gas chromatography-negative chemical ionization-mass spectrometry （GC-NCI-MS）. The analysis conditions for gas chromatography and mass spectrometry were optimized. Then, the samples were extracted by ultrasonication, purified on a Florisil SPE column, monitored in the selective ion monitoring （SIM） scanning mode, and quantified by the external standard method. With this method, a good linear relationship was found over a wide mass concentration range from 0.0501 to 100.17 mg/L, with a linear correlation coefficient （R2） of 0.9995. The detection limit for SCCPs by this method was found to be as low as 0.50 μg/g （i. e. 0.000050%） and the average recoveries for SCCPs spiked in the blank samples varied from 83.2% to 96.3% with relative standard deviations （RSDs） of 1.56%-6.02%. Ten batches of samples were tested and the contents of SCCPs detected in each batch were in the range from 0.016% to 0.55%, which agrees well the European Union limitation requirement for SCCPs. Thus, this method is suitable for qualitative and quantitative analyses of SCCPs in synthetic surfacing layers used in sports and diluents.