Wang Jing, Pan Hefang, Liu Zhengzheng, Ge Fei
Zhejiang Province Environmental Monitoring Centre, Hangzhou, Zhejiang, China.
J Chromatogr A. 2009 Mar 20;1216(12):2499-503. doi: 10.1016/j.chroma.2009.01.062. Epub 2009 Jan 24.
A novel method has been developed for the determination of alkylphenols in soil by ultra-high-pressure liquid chromatography employing small particle sizes, combined with tandem mass spectrometry. Soil samples were extracted with pressurized liquid extraction (PLE) and then cleaned with solid-phase extraction (SPE). The extracts were separated on C18 column (1.7 microm, 50 mm x 2.1mm) with a gradient elution and a mobile phase consisting of water and acetonitrile, and then detected by an electrospray ionization tandem mass spectrometry in negative ion mode with multiple reaction monitoring (MRM). Compared with traditional liquid chromatography, it took ultra-high-pressure liquid chromatography much less time to analyze alkylphenols. Additionally, the ultra-high-pressure liquid chromatography/tandem mass spectrometry method produces satisfactory reliability, sensitivity, and accuracy. The average recoveries of the three target analytes were 74.0-103.4%, with the RSD<15%. The calibration curves for alkylphenols were linear within the range of 0.01-0.4 microg/ml, with the correlation coefficients greater than 0.99. When 10 g soil sample was used for analysis, the limits of quantification (LOQs) of the three alkylphenols were all 1.0 microg/kg.
已开发出一种新方法，采用小粒径超高压液相色谱结合串联质谱法测定土壤中的烷基酚。土壤样品通过加压液体萃取（PLE）进行萃取，然后通过固相萃取（SPE）进行净化。萃取物在C18柱（1.7微米，50毫米×2.1毫米）上进行分离，采用梯度洗脱，流动相由水和乙腈组成，然后通过电喷雾电离串联质谱在负离子模式下进行多反应监测（MRM）检测。与传统液相色谱相比，超高压液相色谱分析烷基酚所需时间大大缩短。此外，超高压液相色谱/串联质谱法具有令人满意的可靠性、灵敏度和准确性。三种目标分析物的平均回收率为74.0 - 103.4%，相对标准偏差（RSD）<15%。烷基酚的校准曲线在0.01 - 0.4微克/毫升范围内呈线性，相关系数大于0.99。当使用10克土壤样品进行分析时，三种烷基酚的定量限（LOQ）均为1.0微克/千克。
