Van Hoi Bui, Vu Cam-Tu, Phung-Thi Lan-Anh, Thi Nguyen Thao, Nguyen Phuong Thanh, Mai Huong, Le Phuong-Thu, Nguyen Thanh-Hien, Thanh Duong Dao, Nguyen Thi Hue, Le-Van Dung, Chu Dinh Binh
Department of Water-Environment-Oceanography, University of Science and Technology of Hanoi (USTH), Vietnam Academy of Science and Technology, 18 Hoang Quoc Viet, Cau Giay, Hanoi 100000, Vietnam.
School of Environmental Science and Technology, Hanoi University of Science and Technology, No. 1 Dai Co Viet, Hanoi 100000, Vietnam.
J Anal Methods Chem. 2021 Jan 8;2021:6628285. doi: 10.1155/2021/6628285. eCollection 2021.
In this study, an analytical method for the simultaneous determination of 7 major pharmaceutical residues in Vietnam, namely, carbamazepine, ciprofloxacin, ofloxacin, ketoprofen, paracetamol, sulfamethoxazole, and trimethoprim, in surface water and hospital wastewater has been developed. The method includes enrichment and clean-up steps by solid phase extraction using mix-mode cation exchange, followed by identification and quantification using an ultrahigh-performance liquid chromatography and tandem mass spectrometry and employing electrospray ionization (UPLC-ESI-MS/MS). Seven target compounds were separated on the reversed phase column and detected in multiple reaction monitoring (MRM) mode within 6 minutes. The present study also optimized the operating parameters of the mass spectrometer to achieve the highest analytical signals for all target compounds. All characteristic parameters of the analytical method were investigated, including linearity range, limit of detection, limit of quantification, precision, and accuracy. The important parameter in UPLC-ESI-MS/MS, matrix effect, was assessed and implemented via preextraction and postextraction spiking experiments. The overall recoveries of all target compounds were in the ranges from 55% to 109% and 56 % to 115% for surface water and hospital wastewater, respectively. Detection limits for surface water and hospital wastewater were 0.005-0.015 g L and 0.014-0.123 g L, respectively. The sensitivity of the developed method was allowed for determination of target compounds at trace level in environmental water samples. The in-house validation of the developed method was performed by spiking experiment in both the surface water and hospital wastewater matrix. The method was then applied to analyze several surface water and hospital wastewater samples taken from West Lake and some hospitals in Vietnam, where the level of these pharmaceutical product residues was still missed. Sulfamethoxazole was present at a high detection frequency in both surface water (33% of analyzed samples) and hospital wastewater (81% of analyzed samples) samples.
在本研究中，已开发出一种同时测定越南地表水中和医院废水中7种主要药物残留的分析方法，这7种药物分别是卡马西平、环丙沙星、氧氟沙星、酮洛芬、对乙酰氨基酚、磺胺甲恶唑和甲氧苄啶。该方法包括采用混合模式阳离子交换的固相萃取进行富集和净化步骤，随后使用超高效液相色谱和串联质谱并采用电喷雾电离（UPLC-ESI-MS/MS）进行鉴定和定量。7种目标化合物在反相柱上分离，并在6分钟内以多反应监测（MRM）模式进行检测。本研究还优化了质谱仪的操作参数，以实现所有目标化合物的最高分析信号。研究了该分析方法的所有特征参数，包括线性范围、检测限、定量限、精密度和准确度。通过萃取前和萃取后加标实验评估并实施了UPLC-ESI-MS/MS中的重要参数——基质效应。所有目标化合物在地表水中的总回收率为55%至109%，在医院废水中为56%至115%。地表水和医院废水的检测限分别为0.005 - 0.015 μg/L和0.014 - 0.123 μg/L。所开发方法具有的灵敏度能够测定环境水样中痕量水平的目标化合物。通过在地表水和医院废水基质中进行加标实验，对所开发方法进行了内部验证。然后将该方法应用于分析从越南西湖和一些医院采集的多个地表水和医院废水样本，此前这些药物残留的水平一直未被检测到。磺胺甲恶唑在地表水（占分析样本的33%）和医院废水（占分析样本的81%）样本中的检测频率都很高。
