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Method Validation for the Trace Analysis of Geosmin and 2-Methylisoborneol in Water by and#195;and#162;and#194;and#8364;and#194;and#339;Salt-Freeand#195;and#162;and#194;and#8364;and#194;and#157; Purge-and-Trap Sampling/GC-MS, Using the Eclipse 4660 Sample Concentrator | Abstract
ISSN: 2157-7587

Hydrology: Current Research
Open Access

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Research Article

Method Validation for the Trace Analysis of Geosmin and 2-Methylisoborneol in Water by “Salt-Free” Purge-and-Trap Sampling/GC-MS, Using the Eclipse 4660 Sample Concentrator

Thavrin Manickum* and Wilson John
Scientific Services Laboratories, Engineering & Scientific Services, Heald Office, Level 3, Umgeni Water, 310 Burger Street, Pietermaritzburg 3201, KwaZulu-Natal, South
Corresponding Author : Thavrin Manickum
Scientific Services Laboratories
Engineering & Scientific Services
Head Office, Level 3, Umgeni Water
310 Burger Street, Pietermaritzburg 3201
KwaZulu-Natal, South Africa
Tel: +27 33 341 1067
Fax: +27 33 341 1501
E-mail: [email protected]
Received March 27, 2012; Accepted May 23, 2012; Published May 30, 2012
Citation: Manickum? T, John W (2012) Method Validation for the Trace Analysis of Geosmin and 2-Methylisoborneol in Water by “Salt-Free” Purge-and-Trap Sampling/GC-MS, Using the Eclipse 4660 Sample Concentrator. Hydrol Current Res 3:134. doi: 10.4172/2157-7587.1000134
Copyright: © 2012 Manickum? T, et al. This is an open-access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.
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Abstract

The Eclipse 4660 purge-and trap sample concentrator, coupled to a gas chromatograph-mass spectrometer, was fully validated for trace analysis of the taste-odorants geosmin (GSM) and 2-methylisoborneol (2-MIB) in the absence of salt or methanol. The procedure involved purging a 25 mL sample volume, at 80°C, for 11 min. Quantitation was done by separation on an HP 5-MS capillary column (30 m × 0.25 mm × 0.25 μm), followed by mass spectrometric detection in the selected ion monitoring (SIM) mode. The method was found to be linear (r2 ≥ 0.995) over the calibration range 0-100 ng/L for both target analytes. The overall accuracy, determined by recovery, was 104.21% ± 19.46 (mean ± SD, range = 65.29-143.13%) for 2-MIB, and 85.24% ± 8.28 (mean ± SD, range = 68.66-101.82%) for GSM. The within-day precision averaged 7.97% for 2-MIB, and 8.77% for GSM. The day-to-day precision was 20.96% for 2-MIB, and 7.52% for GSM. The limit of quantitation (LOQ) was 6 ng/L and 5 ng/L for 2-MIB and GSM; the limit of detection (LOD) was 5 ng/L and 4 ng/L for 2-MIB and GSM respectively. Earlier findings regarding the dehydration of 2-MIB to 2-methyl-2-bornene (2-M-2-B) were confirmed. The average amount of 2-M-2-B formed was 27% (range: 15-50%), with RSD = 33.26%. There is evidence of dehydration of 2-MIB to 2-M-2-B at sample purge temperature of 40°C and higher. The poor day-to-day precision for 2-MIB has been proposed to be due to the inconsistent amount of 2-M-2-B formed. A minimum sample purge temperature of 40°C is required to purge 2-MIB and GSM from water, which can be detected by GC/MS under the purge-and-trap conditions at a concentration of 100 ng/L. The developed method was found to be sensitive, accurate, precise and reproducible for trace analysis of geosmin in water matrices.

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