Simple determination of hydrazine in waste water by headspace solid-phase micro extraction and gas chromatography-tandem mass spectrometry after derivatization with trifluoro pentanedione

다국어 초록 (Multilingual Abstract)

<P><B>Abstract</B></P> <P>A headspace solid-phase micro extraction (HS-SPME) and gas chromatography-tandem mass spectrometric (GC-MS/MS) method is described to detect hydrazine after derivatization with 1,1,1-trifluoro-2,4-pentanedione (1,1,1-TFPD) to 3-methyl-5-(trifluoromethyl) pyrazole in industrial waste water. The following optimal HS-SPME conditions were used: 85 μm-carboxen-polydimethylsiloxane fibre, 100 mg L<SUP>−1</SUP> TFPD, saturated NaCl, an extraction/derivatization temperature of 80 °C, a heating time of 40 min, and a pH of 9.5. Under the established conditions, the detection and quantification limits were 0.002 μg L<SUP>−1</SUP> and 0.007 μg L<SUP>−1</SUP> by using 5 mL of waste water and the intra- and inter-day relative standard deviations were less than 10.2% at concentrations of 0.02 and 0.1 μg L<SUP>−1</SUP>. The calibration curve showed good linearity, with <I>r</I> <SUP>2</SUP> = 0.998; the accuracy was in the range of 98.0–103%; and the precision of the assay was less than 10.2% in industrial waste water. Hydrazine was detected over a concentration range of 0.011–0.074 μg L<SUP>−1</SUP> in 5 of 20 waste water samples.</P> <P><B>Highlights</B></P> <P> <UL> <LI> New single peak derivatization method of hydrazine with 1,1,1-trifluoro-2,4-pentanedione in wastewater for HS-SPME. </LI> <LI> Easy manipulation and amenable to automation. </LI> <LI> This method requires no solvent for sample extraction and is environmentally friendly. </LI> <LI> This method shows low interference due to the use of HS-GC-MS/MS. </LI> </UL> </P> <P><B>Graphical abstract</B></P> <P>[DISPLAY OMISSION]</P>