Simultaneous determination of five estrogens and four androgens in water samples by online solid-phase extraction coupled with high-performance liquid chromatography–tandem mass spectrometry

Abstract

a b s t r a c tA novel method for simultaneous determination of five estrogens and four androgens by online solid-phase extraction (SPE) coupled with high-performance liquid chromatography-tandem mass spectrometry (HPLC-ESI-MS/MS) in water samples was developed. An aliquot of 50 mL water sample after filtration was injected directly into autosampler and the analytes were preconcentrated on a NG1 online SPE column. After cleanup step the analytes were eluted in back flush mode and then separated on a liquid chromatography column. The experimental parameters, such as sample loading flow rate, cleanup condition and elution time, were optimized in detail. Estrogens and androgens were detected in negative and positive mode, respectively. High ionization efficiency of all the analytes was achieved by adding of 1‰ ammonia in the mobile phase. The recoveries ranged from 31.8% to 119.0% and the inter-day RSDs ranged from 2.7% to 19.6%. The limits of detections (LODs) were between 0.1 and 2.5 ng/L. The proposed method was successfully applied to the analysis of three types of water samples, including river water, influent and effluent water from a wastewater treatment plant (WWTP). The recoveries of androgens were not that good and a further study is being planned to improve the sensitivity for them. The proposed method is simple, sensitive and suitable for simultaneous analysis and monitoring of estrogens and androgens in water samples.

Direct analysis of eight chlorophenols in urine by large volume injection online turbulent flow solid-phase extraction liquid chromatography with multiple wavelength ultraviolet detection

“…The setup and method procedures are similar to our previous study [38]. Briefly, five major steps were used: sampling, cleanup, SPE column regeneration, elution and HPLC separation.…”

An on-line solid phase extraction–liquid chromatography tandem mass spectrometry method for the determination of perfluoroalkyl substances in the Antarctic ice core samples

“…Consequently, this technique could considerably enrich analyte and significantly improve the sensitivity using a limited volume of sample, which is important for the analysis of trace components in extremely valuable samples in remote areas, such as Antarctic and Arctic areas. Therefore, the on-line extraction technique has been rapidly developed and widely used in the analysis of a variety of contaminants in environmental and biological samples since it was invented [13][14][15]. However, to the best of our knowledge, the analysis of perfluoroalkyl substances using on-line solid-phase extraction technique has been rarely reported.…”

Quantitative mass spectrometry methods for pharmaceutical analysis

“…Furthermore, sample preparation is fully automated making this set-up more robust in comparison with offline SPE. Although recovery rates mainly depend on the type of sorbent, the loading speed is also very important to obtain good recoveries [138]. Ideal recoveries approach 100%, but according to the ICH guidelines, recoveries between 80% and 120% are considered acceptable [63,139,140].…”