Determination of 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce by headspace derivatization solid-phase microextraction combined with gas chromatography-mass spectrometry.
This study proposes a method for identifying 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous matrices by using headspace on-fiber derivatization following solid-phase microextraction combined with gas chromatography-mass spectrometry. The optimized SPME experimental procedures for extracting 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous solutions involved a 85 microm polyacrylate-coated fiber at pH 6, a sodium chloride concentration of 0.36 g mL(-1), extraction at 50 degrees C for 15 min and desorption of analytes at 260 degrees C for 3 min. Headspace derivatization was conducted in a laboratory-made design with N-methyl-N-(trimethylsilyl)-trifluoroacetamide vapor following solid-phase microextraction by using 3 microL N-methyl-N-(trimethylsilyl)-trifluoroacetamide at an oil bath temperature of 230 degrees C for 40 s. This method had good repeatability (R.S.D.s < or = 19%, n = 8) and good linearity (r2 > or = 0.9972) for ultrapure water and soy sauce samples that were spiked with two analytes. Detection limits were obtained at the ng mL(-1). The result demonstrated that headspace on-fiber derivatization following solid-phase microextraction was a simple, fast and accurate technique for identifying trace 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce.
Lee
Maw-Rong
MR
Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan, ROC. mrlee@dragon.nchu.edu.tw
Chiu
Tzu-Chun
TC
Dou
Jianpeng
J
D008401:Gas Chromatography-Mass Spectrometry; D009153:Mutagens / Q000032:analysis; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods; D045730:Soy Foods / Q000032:analysis*; D000517:alpha-Chlorohydrin / Q000031:analogs & derivatives* / Q000032:analysis*
D009153:Mutagens; C033489:1,3-dichloro-2-propanol; D000517:alpha-Chlorohydrin