A Convenient Method for Epichlorohydrin Determination in Water Using Headspace-Solid-Phase Microextraction and Gas Chromatography

Lasa, Maitena; Garcı́a, Rosa; Millán, Esmeralda

doi:10.1093/chromsci/44.7.438

Cited by 12 publications

(13 citation statements)

References 9 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Data from Tomlin (2000) Food Anal. Methods (2011) 4:293-299 On the basis of the literature and the experience of the laboratory, different variables were selected to define the experimental field in the SPME procedure (Beltran et al 2000;Zambonin et al 2002;Lasa et al 2006;López et al 2007;Cortés-Aguado et al 2008;Zuazagoitia et al 2009). …”

Section: Resultsmentioning

confidence: 99%

Optimization of Solid-Phase Microextraction Procedure Coupled to GC-ECD for Triazole Fungicides Determination in Juice Samples

2010

View full text Add to dashboard Cite

A solid-phase microextraction (SPME) procedure followed by gas chromatography electron capture detection (GC/ECD) for the determination of triazole residues was developed. An experimental design with two steps was done. Firstly, a 2 6−2 fractional factorial design for screening several experimental variables (fiber-coating type, extraction temperature, extraction time, stirring rate, desorption temperature, and desorption time) was done. After, a twofactor central composite design for optimizing, the experimental conditions were carried out. The chosen experimental conditions were: fiber, PDMS/DVB; extraction time, 45 min; extraction temperature, 60°C; desorption time, 3 min; desorption temperature, 260°C, and stirring speed, 500 rpm. Using those conditions the limits of detection obtained for tetraconazole, myclobutanil, and diniconazole were in the order of few μg L −1 in grape and apple liquid extracts. Recoveries were from 93.6% to 112.1%. Relative standard deviation ranged from 1.2% to 11.6% (apple) and 6.7 to 18.0% (grape). The method was applied to five grape samples and 13 apple samples collected in Navarra, Rioja, and Basque Country. Quantification was performed by the standard addition method. Three standard additions by duplicate covering adequate range concentration were used. Myclobutanil was found in three apple samples (110-122 μg L −1 ) and diniconazole in one grape sample (9.4 μg L −1 ).

show abstract

Section: Resultsmentioning

confidence: 99%

Optimization of Solid-Phase Microextraction Procedure Coupled to GC-ECD for Triazole Fungicides Determination in Juice Samples

2010

View full text Add to dashboard Cite

show abstract

“…ECH, similarly to other volatile organic compounds, has been determined in water by gas chromatography (GC), although this can require multi‐stage and time‐consuming procedures prior to the chromatographic analysis. The methods involved are most often based on isolation and/or enrichment techniques as dynamic headspace purge and trap,6, 7 static headspace,7, 8 liquid‐liquid extraction (LLE),8 solid‐phase extraction (SPE),5, 8 or solid‐phase microextraction (SPME) 8–10. GC determination has been carried out by using detection systems as electron capture detection (ECD),5, 7, 9, 12 flame ionization detection (FID)9, 10, 12 and mass spectrometry (MS) 10–13…”

mentioning

confidence: 99%

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

Ripollés

Marín

López

et al. 2009

Rapid Comm Mass Spectrometry

View full text Add to dashboard Cite

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)

show abstract

“…From the literature review there were few analytical methods which have been reported for Epichlorohydrin such as GC methods [8] …”

Section: Rivaroxaban Is Chemically 5-chloro-n-({(5s)-2-oxo-3-[4-(3-oxmentioning

confidence: 99%

Enantiomeric Separation of S-Epichlorohydrin and R-Epichlorohydrin by Capillary Gas Chromatography with FID Detector

Kumar¹,

Vasa²,

Kumar³

et al. 2016

AJAC

View full text Add to dashboard Cite

The aim of this study was to develop a simple and derivatization free method for the Quantification of S-Epichlorohydrin in R-Epichlorohydrin by using a gas chromatography coupled with flame ionization detector (FID). Enantiopure epichlorohydrin was a valuable epoxide key starting material for preparing optically active Rivaroxaban. The enantiomeric separations of S-Epichlorohydrin and R-Epichlorohydrin were achieved on Gamaa-Dex-225 (30 meters × 0.25 mm I.D, 0.25 µm) column with a total run time of 30 min. Nitrogen was used as a carrier gas with constant pressure 25.0 psi. The critical experimental parameters such as, column selection, flow rate, injection volume and diluent were studied and optimized. Excellent correlation coeffient between peak responses and concentrations was >0.9998. The recoveries of S-Epichlorohydrin spiked in R-Epichlorohydrin were in the range from 98.2% to 102.8%. Limit of quantitation for S-Epichlorohydrin was sufficiently lower than limits specified by ICH. The method has validated as per International Conference on Harmonization (ICH) guidelines. A precise, accurate, linear and robust Gas Chromatography method was developed for the quantification of S-Epichlorohydrin in R-Epichlorohydrin for Rivaroxaban.

show abstract

A Convenient Method for Epichlorohydrin Determination in Water Using Headspace-Solid-Phase Microextraction and Gas Chromatography

Cited by 12 publications

References 9 publications

Optimization of Solid-Phase Microextraction Procedure Coupled to GC-ECD for Triazole Fungicides Determination in Juice Samples

Optimization of Solid-Phase Microextraction Procedure Coupled to GC-ECD for Triazole Fungicides Determination in Juice Samples

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

Enantiomeric Separation of S-Epichlorohydrin and R-Epichlorohydrin by Capillary Gas Chromatography with FID Detector

Contact Info

Product

Resources

About