Identificación y cuantificación de contaminantes emergentes en aguas residuales por microextracción en fase sólida-cromatografía de gases-espectrometría de masas (MEFS-CG-EM)

Araceli Peña-Álvarez, Alejandra Castillo-Alanís
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引用次数: 29

Abstract

A methodology by SPME-GC-MS was developed and optimized for the simultaneous determination of pharmaceutical and personal care products (PPCP's) in wastewater: ibuprofen, naproxen, chlorofen, triclosan and bisphenol A. The extraction of analytes was performed by SPME using a fiber of PEG (Polietylenglycol), stirring of 1,200 rpm, 30 min extraction time at ambient temperature, 50% NaCl, pH=3 and derivatization on fiber with MTBSTFA (N-methyl-N-tert-butyl-dimethylsilil-trifluoroacetamide). The identification of the analytes was done by comparison of the retention times and the mass spectrum of standards. The quantification was done by selective ion monitoring (SIM) mode. The developed method shown acceptable linearity in the range of 1.0-118.90 pg/mL for ibuprofen, 48.0-1488 pg/mL for naproxen, 4.40-140.8 pg/mL for triclosan, 1.0-58.32 pg/mL for chlorofen, and 1.0-59.16 pg/mL for bisphenol A, all of them with correlation coefficients > 0.99. Several water samples from influents and effluents were analyzed from three wastewater treatment plants in the south of the Mexico City: “University”, “Coyoacan” and “Cerro de la Estrella” all of them belong to the water system of Mexico City. It was shown in this work that SPME is a sample preparation technique that is simple, reproducible, sensitive and fast because it reduces the steps by extracting and simultaneously concentrating the analytes without the use of organic solvents.

固相微萃取-气相色谱-质谱法(MEFS-CG-EM)对废水中新出现污染物的鉴定和定量
建立并优化了SPME- gc - ms同时测定废水中布洛芬、萘普生、氯芬、三氯生和双酚A等药品和个人护理用品(PPCP)的方法。SPME采用聚乙二醇(PEG)纤维,搅拌1200转/分,室温,50% NaCl, pH=3,提取时间30 min,在MTBSTFA (n -甲基- n -叔丁基-二甲基硅烷-三氟乙酰胺)纤维上衍生。通过保留时间和标准品质谱的比较对分析物进行鉴定。定量采用选择性离子监测(SIM)模式。布洛芬在1.0 ~ 118.90 pg/mL、萘普生在48.0 ~ 1488 pg/mL、三氯生在4.40 ~ 140.8 pg/mL、氯芬在1.0 ~ 58.32 pg/mL、双酚A在1.0 ~ 59.16 pg/mL范围内呈良好的线性关系,相关系数均为>0.99. 对墨西哥城南部“大学”、“Coyoacan”和“Cerro de la Estrella”三个污水处理厂的进水和出水水样进行了分析,它们都属于墨西哥城的供水系统。实验结果表明,SPME在不使用有机溶剂的情况下,减少了样品提取和浓缩的步骤,是一种简单、可重复性好、灵敏度高、速度快的样品制备技术。
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