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 µg L⁻¹ and 0.014–0.123 µg L⁻¹, 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.

中文翻译：

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UPLC-MS / MS方法测定药物残留：在地表水和医院废水中的验证和应用

在这项研究中，开发了一种同时测定地表水和医院废水中的7种主要药物残留物的分析方法，该残留物是卡马西平，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。该方法包括以下步骤：通过使用混合模式阳离子交换的固相萃取进行富集和净化步骤，然后使用超高效液相色谱和串联质谱法以及电喷雾电离（UPLC-ESI-MS / MS）进行鉴定和定量。在反相色谱柱上分离了七个目标化合物，并在6分钟内以多反应监测（MRM）模式进行了检测。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，精密度和准确性。UPLC-ESI-MS / MS中的重要参数基质效应是通过提取前和提取后加标实验进行评估和实施的。对于地表水和医院废水，所有目标化合物的总回收率分别为55％至109％和56％至115％。地表水和医院废水的检出限为0.005-0.015 精度和准确性。UPLC-ESI-MS / MS中的重要参数基质效应是通过提取前和提取后加标实验进行评估和实施的。对于地表水和医院废水，所有目标化合物的总回收率分别为55％至109％和56％至115％。地表水和医院废水的检出限为0.005-0.015 精度和准确性。UPLC-ESI-MS / MS中的重要参数基质效应是通过提取前和提取后加标实验进行评估和实施的。对于地表水和医院废水，所有目标化合物的总回收率分别为55％至109％和56％至115％。地表水和医院废水的检出限为0.005-0.015 μ克L- ^-1和0.014-0.123  μ克L- ^-1，分别。所开发方法的灵敏度可用于测定环境水样品中痕量水平的目标化合物。通过对地表水和医院废水基质进行加标实验，对开发的方法进行了内部验证。然后将该方法用于分析从西湖和越南一些医院采集的一些地表水和医院废水样本，这些地方的药物产品残留量仍然漏检。地表水（所分析样品的33％）和医院废水（所分析样品的81％）中均存在高检测频率的磺胺甲恶唑。