Althakafy Jalal T, Kulsing Chadin, Grace Michael R, Marriott Philip J
Australian Centre of Research on Separation Science, School of Chemistry, Faculty of Science, Monash University, Clayton, VIC 3800, Australia; Department of Chemistry, Faculty of Applied Sciences, Umm Al-Qura University, 21955 Makkah, Saudi Arabia.
Australian Centre of Research on Separation Science, School of Chemistry, Faculty of Science, Monash University, Clayton, VIC 3800, Australia.
J Chromatogr A. 2017 Sep 15;1515:164-171. doi: 10.1016/j.chroma.2017.08.003. Epub 2017 Aug 3.
This study developed an analytical approach for sub-ppb level detection and confirmation of 13 pharmaceuticals and personal care products (PPCPs) in water samples using ultra high pressure liquid chromatography hyphenated with a quadrupole Orbitrap mass spectrometer (UHPLC- Q-Orbitrap-MS). Sample preparation was performed by using solid phase extraction (SPE) employing hydrophilic-lipophilic balance cartridges, with elution of sorbed analytes using methanol. Acceptable automatic gain control (AGC) target and maximum injection time (IT) were 1×10 and 200ms, respectively, resulting in a mass accuracy <2ppm. High response signals with sufficient data points per peaks (20-30) were obtained whilst maintaining high resolution of approximately 70,000 full width at half maximum. Extracted ion chromatograms provided quantitative analysis with linearity (R) ranging from 0.9875 to 0.9993 and method detection limits ranging from 0.01-0.61ngmL. Compounds were further analysed by MS/MS analysis, with the MS operated in parallel reaction monitoring (PRM) mode under precursor ion analysis intervals and collision energies chosen for the different PPCPs. The developed method was applied to analyse water samples obtained from sources in Victoria, Australia.
本研究开发了一种分析方法，用于使用超高压液相色谱与四极杆轨道阱质谱仪联用（UHPLC-Q-Orbitrap-MS）对水样中13种药品和个人护理产品（PPCPs）进行亚ppb水平的检测和确证。样品制备采用亲水亲脂平衡柱进行固相萃取（SPE），用甲醇洗脱吸附的分析物。可接受的自动增益控制（AGC）目标和最大进样时间（IT）分别为1×10和200ms，质量精度<2ppm。在保持约70,000的半高宽高分辨率的同时，获得了每个峰具有足够数据点（20-30个）的高响应信号。提取离子色谱图提供了定量分析，线性度（R）范围为0.9875至0.9993，方法检测限范围为0.01-0.61ng/mL。通过MS/MS分析进一步分析化合物，MS在平行反应监测（PRM）模式下运行，根据不同PPCPs选择前体离子分析间隔和碰撞能量。所开发的方法应用于分析从澳大利亚维多利亚州的水源采集的水样。
