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Frontiers of Environmental Science & Engineering

Front. Environ. Sci. Eng.    2016, Vol. 10 Issue (3) : 477-481
Trace analysis of off-flavor/odor compounds in water using liquid-liquid microextraction coupled with gas chromatography—positive chemical ionization-tandem mass spectrometry
Jian LU1,Paul S. WILLS2,P. CHRIS WILSON1,*()
1. Indian River Research and Education Center, University of Florida/IFAS, 2199 South Rock Road, Fort Pierce, FL 34945-3138, USA
2. Harbor Branch Oceanographic Institute at Florida Atlantic University, 5600 U.S. 1 North, Fort Pierce, FL 34946, USA
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A rapid, inexpensive and laboratory friendly method was developed for analysis of off-flavor/odor compounds in fresh and salt water using gas chromatography with chemical ionization-tandem mass spectrometry. Off-flavor/odor compounds included geosmin, 2-methylisoborneol (MIB), 2-isobutyl-3-methyoxypyrazine (IBMP), and 2-isopropyl-3-methoxypyrazine (IPMP). Using this method, a single sample can be extracted within minutes using only 1 mL of organic solvent. The ion transitions for IPMP, IBMP, MIB, and geosmin were 153>121, 167>125, 152>95, and 165>109, respectively. The linearity of this method for analyzing MIB ranged from 4 to 200 ng·L-1, and from 0.8 to 200 ng·L-1 for the other analytes. Method recoveries ranged from 97% to 111% and percent relative standard deviations ranged from 3% to 9%, indicating that the method is accurate, precise, and reliable.

Keywords off-flavor/odor compounds      liquid-liquid microextraction      gas chromatography-tandem mass spectrometry     
Corresponding Authors: P. CHRIS WILSON   
Online First Date: 13 October 2015    Issue Date: 05 April 2016
 Cite this article:   
Jian LU,Paul S. WILLS,P. CHRIS WILSON. Trace analysis of off-flavor/odor compounds in water using liquid-liquid microextraction coupled with gas chromatography—positive chemical ionization-tandem mass spectrometry[J]. Front. Environ. Sci. Eng., 2016, 10(3): 477-481.
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compounds retention time /min precursor ion /(m·z-1) resonant excitation voltage/V quantitative ions/(m·z-1) secondary ions/(m·z-1)
IPMP 8.79 153 0.80 121 83, 138
IBMP 10.28 167 0.62 125 135
MIB 10.58 152 0.44 95 81
TCA (surrogate) 12.60 211 0.93 196 176
Geosmin 13.86 165 0.53 109 95
Tab.1  Operational parameters for the tandem mass spectrometer scans for off-flavor/odor compounds and the surrogate
Fig.1  Typical mass spectra for geosmin, MIB, IBMP, and IPMP
Fig.2  Typical chromatogram from a spiked nano-pure water sample (100 ng·L-1) extracted using the liquid-liquid microextraction method coupled with gas chromatography-positive chemical ionization tandem mass spectrometry analysis
Fig.3  Effect of water types (fresh vs. salt) on peak intensity of target off-flavor/odor compounds. Each analyte was spiked at the concentration of 100 ng·L-1
compound matrix range/(ng·L-1) R2 MDL /(ng·L-1) MQL /(ng·L-1)
Geosmin fresh water 0.8-200 0.999 0.2 0.6
sea water 0.8-200 0.993 0.2 0.6
MIB fresh water 4-200 0.999 1.2 3.6
sea water 4-200 0.998 1.2 3.6
IBMP fresh water 0.8-200 0.992 0.1 0.3
sea water 0.8-200 0.993 0.1 0.3
IPMP fresh water 0.8-200 0.997 0.2 0.6
sea water 0.8-200 0.994 0.2 0.6
Tab.2  Linear range and method detection limits for off-flavor/odor compounds
compounds % recovery (% RSD)
fresh water sea water
IPMP 109 (5) 111 (5)
IBMP 109 (3) 107 (3)
MIB 106 (9) 97 (9)
Geosmin 102 (4) 104 (9)
Tab.3  Recovery of off-flavor/odor compounds from fresh water and sea water
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