Food and Environmental Safety Research Group, Faculty of Pharmacy, University of Valencia, Av. Vicent Andrés Estellés, 46100 Burjassot, Valencia, Spain.
J Chromatogr A. 2012 Jun 29;1244:88-97. doi: 10.1016/j.chroma.2012.04.056. Epub 2012 May 8.
In this work, the performance of ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and capillary liquid chromatography-mass spectrometry (CLC-MS) has been studied for the analysis of eighteen perfluorinated compounds in water samples. UHPLC-MS/MS and CLC-MS analysis were carried out using a Zorbax C-18 column (50 mm × 2.1 mm, 1.8 μm) and a Zorbax SB-C18 column (150 mm × 0.5 mm, 3.5 μm), respectively, in gradient elution mode with a mobile phase of ammonium formate and methanol. Both techniques were compared with conventional LC-MS/MS in terms of speed, sensitivity, selectivity and resolution. Water samples were extracted by solid phase extraction (SPE). Mean absolute recoveries at two concentration levels, 6 and 60 ng L⁻¹, calculated from the eighteen compounds were: 77 ± 12(s) and 82 ± 12(s), respectively. Relative standard deviation (RSD) was lower than 16% for each perfluorinated compound. The results obtained showed that UHPLC-MS/MS and CLC-MS allow the determination of perfluorinated compounds in water samples with satisfactory sensitivity and resolution and reduced analysis time. Therefore, both techniques were employed for the analysis of water samples to determine the target analytes at low concentration levels and with lower analysis times than using HPLC-MS/MS. Similar statistical values were obtained from both techniques at 95% confidence level. Several compounds have been detected, but perfluorooctanoic acid (PFOA) (171 ng L⁻¹ and 148 ng L⁻¹ by UHPLC-MS/MS and CLC-MS, respectively) showed the highest concentration.
在这项工作中,研究了超高效液相色谱-串联质谱(UHPLC-MS/MS)和毛细管液相色谱-质谱(CLC-MS)在水样中十八种全氟化合物分析中的性能。UHPLC-MS/MS 和 CLC-MS 分析分别采用 Zorbax C-18 柱(50mm×2.1mm,1.8μm)和 Zorbax SB-C18 柱(150mm×0.5mm,3.5μm),在梯度洗脱模式下,流动相为甲酸铵和甲醇。从速度、灵敏度、选择性和分辨率等方面比较了这两种技术与传统 LC-MS/MS 的性能。水样通过固相萃取(SPE)进行提取。从十八种化合物中计算出两个浓度水平(6ng/L 和 60ng/L)的平均绝对回收率分别为:77±12(s)和 82±12(s)。每种全氟化合物的相对标准偏差(RSD)均低于 16%。结果表明,UHPLC-MS/MS 和 CLC-MS 能够以令人满意的灵敏度和分辨率,以及缩短分析时间,测定水样中的全氟化合物。因此,这两种技术都用于水样分析,以在较低的分析时间内,以比 HPLC-MS/MS 更低的分析时间来测定低浓度水平的目标分析物。在 95%置信水平下,两种技术均获得了相似的统计值。检测到了几种化合物,但全氟辛酸(PFOA)的浓度最高(UHPLC-MS/MS 和 CLC-MS 分别为 171ng/L 和 148ng/L)。