Simultaneous Determination of 12 Chloroanisoles in Lake Reservoir Waters by Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry

XIONG Mao-fu; REN Min; DU Yi; ZHAO Gao-feng; WANG Xiao-yan

doi:10.15898/j.cnki.11-2131/td.201901210016

XIONG Mao-fu, REN Min, DU Yi, ZHAO Gao-feng, WANG Xiao-yan. Simultaneous Determination of 12 Chloroanisoles in Lake Reservoir Waters by Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry[J]. Rock and Mineral Analysis, 2019, 38(6): 724-733. DOI: 10.15898/j.cnki.11-2131/td.201901210016

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Simultaneous Determination of 12 Chloroanisoles in Lake Reservoir Waters by Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry

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BACKGROUNDChloroanisoles (CAs) are odorous substances and can easily be found in surface waters. The CAs have been found in water environments worldwide. In the food chain, CAs are easily enriched and amplified. The toxicity increases with the number of chlorine atoms substituted. CAs in waters are trace substances which need to be preconcentrated before determination. Previous studies focused on the detection of individual substances.OBJECTIVESTo establish a method which combines headspace solid phase microextraction and gas chromatography-mass spectrometry together, to simultaneously measure 12 CAs in waters.METHODSThe conditions of extraction fiber, temperature, ionic strength, extraction time and stirring rate were compared and optimized in headspace solid phase microextraction. The optimal extraction conditions were confirmed by the results. Extraction temperature was 80℃, ionic strength was 0.35g/mL, extraction time was 40 minutes, stirring rate was 1150r/min, and sample volume was 10mL (15mL extraction bottle).RESULTSQuantitative analysis was performed by gas chromatography-mass spectrometry with selective ion scanning. The linear ranges of the method were 1-50ng/L, and the recoveries were 95.5%-115.1%. The detection limits were 0.045-0.185ng/L and the relative standard deviation was less than 13.02%.CONCLUSIONSCompared with the solid phase extraction and the purge with trap method, this method has a lower detection limit and higher sensitivity of the sample concentration. Also, the precision of the experimental instrument is relatively better than other methods.

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Simultaneous Determination of 12 Chloroanisoles in Lake Reservoir Waters by Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry

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