Determination of Triclosan in Aqueous Samples Using Solid-phase Extraction Followed by On-line Derivatization Gas Chromatography-Mass Spectrometry

Abstract

An efficient and eco-friendly injection-port tert-butyldimethylsilylated (TBDMS) derivatization and gas chromatography-mass spectrometry (GC/MS) were developed to determine an antibacterial agent, triclosan (TCS), and its metabolite: methyltriclosan (MTCS), in wastewater and surface water samples. The effects of several parameters related to the TBDMS-derivatization process (i.e., injection-port temperature, residence time and volume of silylating agent) were investigated. This on-line derivatization-coupled large-volume (10 µL) sample introduction provides sensitive, fast and reproducible results for TCS residue analyses. Each water sample was extracted by reversed-phase C18 solid-phase extraction (SPE) cartridge, and then the recovery efficiency was evaluated using various eluting solutions. Limits of quantitation (LOQs) for MTCS and TCS were 3.0 and 1.0 ng/L in 100 mL of water samples, respectively. Intra- and inter-batch precision with their accuracy were also investigated. The precision for these analytes, as indicated by relative standard deviations (RSDs), proved to be less than 7 and 11%, respectively, for intra- and inter-batch. Accuracy, expressed as the mean recovery, was between 80 and 95%. The method was then applied to environmental water samples, showing the occurrence of TCS in both surface water and municipal wastewater treatment plant (MWTP) influent/effluent samples.

The effect of temperature on Triclosan and Lead exposed mussels

“…Triclosan concentrations in water were measured following Cheng et al (2011) protocol. The extraction was performed with C-18 SPE cartridges (HYPERSEP, 6 ml, 1 g, Thermo Scientific).…”

“…A C C E P T E D M A N U S C R I P T mL of ultrapure water by the use a SPE manifold (Thermo Scientific). Samples were acidified to pH 3 (Cheng et al, 2011), and passed through the cartridges with the aid of vacuum. Then, the cartridges were washed with 4 mL 20 % methanolic solution and air-dried under vacuum for 20 min.…”

Analytical Methodologies for the Determination of Personal Care Products in Water Samples

“…With regard to traditional SPE, different SPE sorbents have been employed depending on the nature of the target compounds, due to the different polarity when comparing triclosan, parabens or isothiazolinones. Thus, non-polar C18 [79,105,122] is used in few cases for triclosan, while PS-DVB modified sorbents [27,37,50,107] or PVP-DVB-based sorbents [28,33,43,67,110,111,115,128] that promote polar and non-polar interactions are preferred when more polar compounds like parabens, isothiazolinones or other PCPs are determined, trying to cover a wide range of retention capacity. It should be mentioned the paper published by Gorga et al [131] who proposed on-line SPE for the determination of different PCPs including some preservatives.…”

“…Thus, it is common to perform a silylation [27,60,103,104,112,122,133], generally after the extraction is accomplished, or acetylation [96,106,116,117,120,123,129,132], generally during the extraction in order to increase both the extraction efficiency and volatility.…”

“…In some cases IT is used [103,122], especially if MS/MS is performed [104,105,113,116,117,119]. In all cases, the ionization is achieved in EI mode.…”