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采用新型 SPE-LC-MS/MS 法检测废水中的抗糖尿病化合物及其一种降解产物。

Sensitive detection of antidiabetic compounds and one degradation product in wastewater samples by a new SPE-LC-MS/MS method.

机构信息

Control Pollution Departament, National Research and Development Institute for Industrial Ecology-ECOIND, Bucharest, Romania.

Faculty of Applied Chemistry and Materials Science, Politehnica University of Bucharest, Bucharest, Romania.

出版信息

J Environ Sci Health A Tox Hazard Subst Environ Eng. 2021;56(3):310-323. doi: 10.1080/10934529.2021.1873671. Epub 2021 Jan 20.

DOI:10.1080/10934529.2021.1873671
PMID:33471573
Abstract

As environment emerging contaminants of anthropogenic origin, antidiabetic drugs are present in the range of high ng/L to ng/mL in the influent and the effluent of the waste water treatment plant (WWTP). The metformin compound is the most used hypoglycemic agent in the world. The aim of this study was to develop a new analytic method, based on solid phase extraction followed by liquid chromatography coupled with mass spectrometric detector (SPE-LC-MS/MS), for identification and quantification of 5 antidiabetic compounds (glibenclamide/glyburide, glimepiride, metformin, glipizide, guanyl urea, gliclazide) and one degradation product (guanyl urea). The investigated environmental samples were the influent and the effluent of four urbans WWTP's. By validating of the analytical method, it was obtained low LOQ's (0.2-4.5 ng/L), satisfactory recovery rates (53.6-116.8%), and corresponding performance parameters: inter-day precision (4.9-8.4%) and reproducibility (11.3-14.6%). The concentrations of antidiabetics were as follow in influent and effluent: metformin 76-2041ng/L and 2-206ng/L, gliclazide (14.1-42.4 ng/L, and 3.3-19.1), glipizide (7.5-11.2 ng/L and 6.5-10ng/L), guanyl urea (6.2-7.3 and 8.3-21.3 ng/L). The efficiency of elimination of the antidiabetics in WWTP's was maximum for metformin (67.6-98.5%), followed, by gliclazide (72.9-78.2%). The lowest elimination efficiency was calculated for glipizide (10.7-13.3%). The guanyl urea undergoes a formation process (74.5-84.2%) in effluent, from the metformin contained in influent.

摘要

作为人为来源的环境新兴污染物,抗糖尿病药物在废水处理厂(WWTP)的进水和出水的浓度范围为高纳克/升至纳克/毫升。二甲双胍是世界上使用最广泛的降血糖药物。本研究旨在开发一种新的分析方法,基于固相萃取(SPE),然后是液相色谱与质谱联用(LC-MS/MS),用于鉴定和定量 5 种抗糖尿病化合物(格列本脲/格列吡嗪、格列美脲、二甲双胍、格列吡嗪、胍基脲、格列齐特)和 1 种降解产物(胍基脲)。所研究的环境样品为四个城市 WWTP 的进水和出水。通过对分析方法的验证,得到了低的检测限(0.2-4.5ng/L)、令人满意的回收率(53.6-116.8%)和相应的性能参数:日内精密度(4.9-8.4%)和重现性(11.3-14.6%)。抗糖尿病药物在进水和出水中的浓度如下:二甲双胍 76-2041ng/L 和 2-206ng/L,格列齐特(14.1-42.4ng/L 和 3.3-19.1),格列吡嗪(7.5-11.2ng/L 和 6.5-10ng/L),胍基脲(6.2-7.3 和 8.3-21.3ng/L)。WWTP 对抗糖尿病药物的去除效率最高的是二甲双胍(67.6-98.5%),其次是格列齐特(72.9-78.2%)。格列吡嗪的去除效率最低(10.7-13.3%)。胍基脲在出水中经历一个形成过程(74.5-84.2%),来自于进水的二甲双胍。

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