Kafeenah Husam I S, Osman Rozita, Bakar N K A
Department of Chemistry, Faculty of Science, University of Malaya 50603 Kuala Lumpur Malaysia
Faculty of Applied Sciences, Universiti Teknologi MARA 40450 Shah Alam Selangor Malaysia.
RSC Adv. 2018 Dec 3;8(70):40358-40368. doi: 10.1039/c8ra06885b. eCollection 2018 Nov 28.
In this work, a new clean-up and pre-concentration method based on disk solid-phase extraction (SPE) was developed to determine multi-class pharmaceutical residues covering a wide range of polarities (log values from -0.5 to 5.1) in water systems, prior to ultra-performance liquid chromatographic-tandem mass spectrometry (UPLC-MS/MS) analyses. Electrospray ionisation in positive and negative modes was used for the simultaneous determination of both acidic and basic pharmaceuticals. The performances of disk SPE and cartridge SPE were compared. The targeted pharmaceutical compounds list included bronchodilators, antidiabetic drugs, antihypertensive drugs, a lipid-lowering agent, analgesics, and anti-inflammatory drugs. Based on our results, the disk SPE demonstrated a higher sensitivity and recovery value and less analysis time as compared to the cartridge SPE method. The limits of detection (LOD) for the new method ranged from 0.02-3.2 ng L, 0.02-3.1 ng L and 0.02-4.7 ng L for tap, effluent and influent wastewater, respectively. The method's absolute recovery values ranged from 70% to 122% for tap water, 62% to 121% for effluent wastewater and 62% to 121% for influent wastewater, except for metformin in which the absolute recovery value was approximately 48% for all samples. Intra-day precision for tap water, effluent and influent wastewater ranged from 3-12%, 4-9% and 2-8%, respectively. The method developed was applied for the determination of targeted pharmaceuticals in tap, effluent, and influent wastewater from one hospital treatment plant in Malaysia. The results revealed that the highest concentrations of certain pharmaceuticals were up to 49 424 ng L (acetaminophen) and 1763 ng L (caffeine) in the influent and effluent wastewater, respectively. The results also showed a variation in the treatment efficiencies for the hospital treatment plant from one compound to another. Nevertheless, the removal efficiencies ranged from 0-99%.
在本研究中，开发了一种基于圆盘固相萃取（SPE）的新型净化和预浓缩方法，用于在超高效液相色谱-串联质谱（UPLC-MS/MS）分析之前，测定水系统中涵盖广泛极性范围（log 值从-0.5至5.1）的多类药物残留。采用正离子和负离子模式的电喷雾电离，用于同时测定酸性和碱性药物。比较了圆盘SPE和柱式SPE的性能。目标药物化合物清单包括支气管扩张剂、抗糖尿病药物、抗高血压药物、一种降脂药物、镇痛药和抗炎药物。基于我们的结果，与柱式SPE方法相比，圆盘SPE表现出更高的灵敏度和回收率，且分析时间更短。新方法的检测限（LOD）对于自来水、出水和进水废水分别为0.02 - 3.2 ng/L、0.02 - 3.1 ng/L和0.02 - 4.7 ng/L。该方法的绝对回收率对于自来水为70%至122%，对于出水废水为62%至121%，对于进水废水为62%至121%，除二甲双胍外，所有样品中其绝对回收率约为48%。自来水、出水和进水废水的日内精密度分别为3 - 12%、4 - 9%和2 - 8%。所开发的方法用于测定马来西亚一家医院污水处理厂的自来水、出水和进水废水中的目标药物。结果表明，某些药物在进水和出水中的最高浓度分别高达49424 ng/L（对乙酰氨基酚）和1763 ng/L（咖啡因）。结果还显示，该医院污水处理厂对不同化合物的处理效率存在差异。然而，去除效率范围为0 - 99%。
