Solid-phase micro-extraction procedure for the determination of 1,3-dichloro-2-propanol in water by on-fibre derivatisation with bis(trimethylsilyl)trifluoroacetamide.
The headspace solid-phase micro-extraction technique with on-fibre derivatisation followed by gas chromatography-tandem mass spectrometry has been evaluated for the analysis of 1,3-dichloro-2-propanol in water. An asymmetric factorial design has been performed to study the influence of five experimental factors: extraction time and temperature, derivatisation time and temperature and pH. The best extraction performance is achieved in the headspace mode, with 5 mL stirred water samples (pH 4) containing 1.3 g of NaCl, equilibrated for 30 min at 25 degrees C, using divinylbenzene-carboxen-polydimethylsiloxane as the fibre coating. On-fibre derivatisation has been used for the first time with 50 microL of bis(trimethylsilyl)trifluoroacetamide at 25 degrees C during 15 min, leading to effective yields. The proposed method provides high sensitivity, good linearity and repeatability (relative standard deviation of 5.1% for 10 ng mL(-1) and n = 5). The limits of detection and quantification were 0.4 and 1.4 ng mL(-1), respectively. Analytical recoveries obtained for different water samples were approx. 100%.
Dpto. de Química Analítica, Nutrición y Bromatología, Facultad de Química, Instituto de Investigaciones y Análisis Alimentarios, Universidad de Santiago de Compostela, Avda. de las Ciencias s/n, 15782, Santiago de Compostela, Spain. tuchi.carro@usc.es
Antonia María
AM
Carro
Paula
P
González
Noelia
N
Fajar
Rosa Antonia
RA
Lorenzo
Rafael
R
Cela
D000081:Acetamides / Q000737:chemistry*; D006863:Hydrogen-Ion Concentration; D015394:Molecular Structure; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052617:Solid Phase Microextraction / Q000379:methods*; D013696:Temperature; D013997:Time Factors; D014297:Trimethylsilyl Compounds / Q000737:chemistry*; D014867:Water / Q000737:chemistry*; D000517:alpha-Chlorohydrin / Q000031:analogs & derivatives* / Q000032:analysis
D000081:Acetamides; C103255:N,O-bis(trimethylsilyl)trifluoroacetamide; D014297:Trimethylsilyl Compounds; D014867:Water; C033489:1,3-dichloro-2-propanol; D000517:alpha-Chlorohydrin