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用于同时定量分析印度南部地表水、地下水和制药废水样品中抗生素残留的超高效液相色谱-串联质谱(UFLC-MS/MS)分析方法的开发与验证

Development and Validation of UFLC-MS/MS Analytical Method for the Simultaneous Quantification of Antibiotic Residues in Surface Water, Groundwater, and Pharmaceutical Waste Water Samples from South India.

作者信息

Kamatham Sravani, Seeralan Manoharan, Sekar Uma, Kuppusamy Sujatha

机构信息

Department of Pharmacology, Sri Ramachandra Faculty of Pharmacy, Sri Ramachandra Institute of Higher Education and Research, (DU), Porur, Chennai 600116, India.

Vaccine Research Centre-Bacterial Vaccine, Centre for Animal Health Studies, TANUVAS, Madhavaram, Chennai 600051, India.

出版信息

ACS Omega. 2024 Mar 6;9(11):12801-12809. doi: 10.1021/acsomega.3c08566. eCollection 2024 Mar 19.

DOI:10.1021/acsomega.3c08566
PMID:38524455
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC10956121/
Abstract

Antibiotic residues in pharmaceutical wastewater pose a significant environmental concern due to their potential role in fostering antimicrobial resistance. South Indian pharmaceutical companies produce a wide range of antibiotics. As a result, the industries that discharge water may include antibiotic residues, which could be harmful to the environment. In this study, a novel, quick, accurate, and sensitive approach for the simultaneous detection of 11 antibiotics was established, and triple quadrupole mass spectrometry, ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS), and selective solid-phase extraction (SPE) were used for validation. Utilizing a mixed mode reversed-phase/cation-exchange cartridge (SPE using Strata X, 33 μm), the single-cartridge extraction procedure was performed and validated. Relative standard deviations for most of the antibiotics ranged from 3.5 to 0.56 with recoveries ranging from 57 to 85%. The samples were injected into the UFLC-MS/MS apparatus at a volume of 10 μL for analysis. The auto sampler cooler temperature was kept at 150 °C, while the column temperature was kept at 40 °C. After validation, the technique was determined to be linear in the range of 2.0-1000.0 ng/mL. The retention period for antibiotics was between 1.2 and 1.5 min. Antibiotics transitions for multiple reaction monitoring| were between 235.1/105.9 and 711.5/467.9 /. The method of analysis took 2.5 min to run completely. Antibiotic residues were efficiently analyzed using the established analytical approach in pharmaceutical wastewater (influent and effluent), surface, and groundwater. Eleven antibiotics were found in the water samples during examination with concentrations ranging between 2.313 and 95.744 ng/L. The procedure was shown to be much more environmentally friendly than other contemporary methods based on the green analytical procedure index's evaluation of greenness. Blue applicability grade index tool indicated the developed method's practicality in comparison with that of other reported method.

摘要

制药废水中的抗生素残留因其在促进抗菌药物耐药性方面的潜在作用而引起了重大的环境问题。印度南部的制药公司生产各种各样的抗生素。因此,排放废水的行业可能含有抗生素残留,这可能对环境有害。在本研究中,建立了一种新颖、快速、准确且灵敏的同时检测11种抗生素的方法,并使用三重四极杆质谱、超快速液相色谱 - 串联质谱(UFLC-MS/MS)和选择性固相萃取(SPE)进行验证。使用混合模式反相/阳离子交换柱(使用Strata X,33μm的SPE)进行单柱萃取程序并进行验证。大多数抗生素的相对标准偏差范围为3.5%至0.56%,回收率范围为57%至85%。将样品以10μL的体积注入UFLC-MS/MS仪器进行分析。自动进样器冷却器温度保持在150°C,而柱温保持在40°C。验证后,该技术在2.0 - 1000.0 ng/mL范围内呈线性。抗生素的保留时间在1.2至1.5分钟之间。多反应监测的抗生素跃迁在235.1/105.9和711.5/467.9之间。分析方法运行完全需要2.5分钟。使用所建立的分析方法对制药废水(进水和出水)、地表水和地下水中的抗生素残留进行了有效分析。在检测过程中,水样中发现了11种抗生素,浓度范围在2.313至95.744 ng/L之间。根据绿色分析程序指数对绿色度的评估,该程序比其他当代方法更加环保。蓝色适用性等级指数工具表明,与其他报道的方法相比,所开发方法具有实用性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d086/10956121/4fc68dc6b284/ao3c08566_0004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d086/10956121/bd80a657d532/ao3c08566_0001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d086/10956121/b8bb0456ae35/ao3c08566_0002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d086/10956121/a694a9a5fabe/ao3c08566_0003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d086/10956121/4fc68dc6b284/ao3c08566_0004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d086/10956121/bd80a657d532/ao3c08566_0001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d086/10956121/b8bb0456ae35/ao3c08566_0002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d086/10956121/a694a9a5fabe/ao3c08566_0003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d086/10956121/4fc68dc6b284/ao3c08566_0004.jpg

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