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采用混合模式固相萃取和液相色谱串联质谱法对环境水样中的沙坦类药物进行选择性测定。

Selective determination of sartan drugs in environmental water samples by mixed-mode solid-phase extraction and liquid chromatography tandem mass spectrometry.

机构信息

Department of Analytical Chemistry, Nutrition and Food Sciences. Institute for Research and Food Analysis (IIAA). Universidade de Santiago de Compostela, 15782, Santiago de Compostela, Spain.

Department of Analytical Chemistry, Nutrition and Food Sciences. Institute for Research and Food Analysis (IIAA). Universidade de Santiago de Compostela, 15782, Santiago de Compostela, Spain.

出版信息

Chemosphere. 2019 Jun;224:562-571. doi: 10.1016/j.chemosphere.2019.02.137. Epub 2019 Feb 27.

Abstract

Herein, a method for the simultaneous determination of the currently prescribed sartan drugs (eprosartan, EPR; olmesartan, OLM; losartan, LOS; candesartan, CAN; telmisartan, TEL; irbesartan, IRB; and valsartan, VAL), and the biodegradation product valsartan acid (VALA), in water samples (raw and treated wastewater, river and tap water) was developed. Solid-phase extraction (SPE) and ultra-performance liquid chromatography (UPLC) tandem mass spectrometry (MS/MS) were employed as concentration and determination techniques, respectively. Different sorbents and elution solvents were tested for sample preparation. Under optimized conditions, samples at neutral pH (6-8 units) were concentrated using mixed-mode (reversed-phase and anionic exchange) cartridges. Thereafter, the sorbent was washed with 5 mL of a methanol: water (1:1) solution, dried under a nitrogen stream and compounds were eluted with 2 mL of methanol: NH (98:2). The accuracy of the method (accounting for SPE efficiency and matrix effects during electrospray ionization) was investigated using solvent-based calibration standards. Global recoveries, obtained for different water matrices (tap, river, treated and raw wastewater), ranged from 82% to 134%, with standard deviations between 2 and 18%. LOQs varied from 2 to 50 ng L. Analysis of un-spiked samples confirmed: (1) the incomplete removal of sartans at sewage treatment plants (STPs), (2) the formation of VALA during municipal water treatment, and (3) the presence of VALA in the processed tap water samples. Additional findings of the current study are the detection of hydroxylated derivatives of the sartan drugs IRB and LOS in wastewater, and the E-Z isomerization of EPR in environmental water samples.

摘要

本文建立了一种同时测定目前规定的沙坦类药物(厄贝沙坦、EPR;奥美沙坦、OLM;氯沙坦、LOS;坎地沙坦、CAN;替米沙坦、TEL;依普罗沙坦、IRB;缬沙坦、VAL)和生物降解产物缬沙坦酸(VALA)在水样(原水和处理后的废水、河水和自来水)中的方法。采用固相萃取(SPE)和超高效液相色谱(UPLC)串联质谱(MS/MS)分别作为浓缩和测定技术。测试了不同的吸附剂和洗脱溶剂用于样品制备。在优化条件下,在中性 pH(6-8 个单位)下,使用混合模式(反相和阴离子交换)柱浓缩样品。然后,用 5ml 甲醇:水(1:1)溶液洗涤吸附剂,用氮气流干燥,用 2ml 甲醇:NH(98:2)洗脱化合物。采用基于溶剂的校准标准研究了方法的准确性(考虑 SPE 效率和电喷雾电离过程中的基质效应)。不同水基质(自来水、河水、处理和原水)的总回收率在 82%至 134%之间,标准偏差在 2%至 18%之间。LOQs 从 2 到 50ng/L 不等。对未加标样品的分析证实:(1)污水处理厂(STP)对沙坦类药物的不完全去除,(2)在城市水处理过程中形成 VALA,以及(3)在处理后的自来水样品中存在 VALA。本研究的其他发现是检测到废水中原沙坦类药物 IRB 和 LOS 的羟基衍生物,以及环境水样中 EPR 的 E-Z 异构化。

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