Determination of sub‐ppb epichlorohydrin levels in water by on‐line solid‐phase extraction liquid chromatography/tandem mass spectrometry

Abstract

8A new sensitive and selective method based on on-line solid-phase extraction (SPE) coupled 9 to LC(ESI)MS/MS using a triple quadrupole analyzer has been developed for the determination of 10 epichlorohydrin (ECH) in different types of water samples. The great difficulties for ECH direct 11 determination resulting from its low molecular size, high polarity and non-easily ionizable molecule 12 make necessary a previous derivatization step. This previous reaction was optimized employing 3,5-13 difluorobenzylamine as derivative agent adding Fe(III) to catalyze the derivatization process. In 14 order to achieve accurate quantification and for correction of matrix effects, losses in the 15 derivatization process and instrumental deviations, ECH isotope labelled (ECH-d 5 ) was added as 16 internal standard (IS) to water samples. The method was validated based on European SANCO 17 guidelines using drinking and other types of treated water spiked at two concentration levels (0.1 18 and 1.0 µg/L), the lowest having been established as the limit of quantification (LOQ)

New Strategy for the Screening of Lysosomal Storage Disorders: The Use of the Online Trapping-and-Cleanup Liquid Chromatography/Mass Spectrometry

“…The DBSs were stored in aluminum bags with desiccant packs. Results suggested that lysosomal enzymes are stable at 4 °C, and no loss activity was noted except for GLA (minus 29.5% if compared to day 0 levels) in agreement with published data (Figures S-2, S-3, and S-4). For the screening purpose, in our center, the median storage time between the drawing of the blood sample and the analysis was 32 h (minimum 20 h, maximum 58 h).…”

“…Many authors used online extraction coupled to LC-MS/MS especially in drug assay applications. 47,48 As far as we know, this is the first use of this analytical approach to detect some LSDs for screening purposes.…”

“…This simple method takes only 4 min as analysis run time and does not involve any time-consuming sample preparation step after the enzymatic reaction. Many authors used online extraction coupled to LC-MS/MS especially in drug assay applications. , As far as we know, this is the first use of this analytical approach to detect some LSDs for screening purposes.…”

Improved solid-phase microextraction extraction procedure to detect trace-level epichlorohydrin in municipal water systems by HS-SPME-GC/MS

“…After the extraction, gas chromatography (GC) with electron-capture detector (ECD), flame ionization detector (FID), or mass spectrometry (GC/MS) are used as the analytical apparatus ( Sarzanini et al, 2000 ; Bruzzoniti et al, 2004 ; Ripollés et al, 2009 ). For example, the German method, Water Quality-Determination of Epichlorohydrin , applies the liquid-solid extraction followed by the GC-MS or GC-ECD, which offers a limit of determination of 0.5 μg/L in routine analysis.…”