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Orthogonal Design Study on Factors Affecting the Determination of Common Odors in Water Samples by Headspace Solid-Phase Microextraction Coupled to GC/MS.

Peng S, Ding Z, Xia W, Zheng H, Xia Y, Chen X - J Anal Methods Chem (2013)

Bottom Line: The optimum was the following: temperatures of extraction and desorption, 65°C and 260°C, respectively; times of extraction and desorption, 30 min and 5 min, respectively; ionic strength, 25% (w/v); rotate-speed, 600 rpm; solution pH, 5.0.Calculated calibration curves gave high levels of linearity with a correlation coefficient value of 0.9999 for them.The RSDs were 2.75%~3.80% and 4.35%~7.6% for geosmin and 2-MIB, respectively, and the recoveries were 91%~107% and 91%~104% for geosmin and 2-MIB, respectively.

View Article: PubMed Central - PubMed

Affiliation: School of Public Health, Southeast University, Nanjing, Jiangsu 210009, China.

ABSTRACT
Geosmin and 2-MIB are responsible for the majority of earthy and musty events related to the drinking water. These two odorants have extremely low odor threshold concentrations at ng L(-1) level in the water, so a simple and sensitive method for the analysis of such trace levels was developed by headspace solid-phase microextraction coupled to gas chromatography/mass spectrometry. In this study, the orthogonal experiment design L32 (4(9)) was applied to arrange and optimize experimental conditions. The optimum was the following: temperatures of extraction and desorption, 65°C and 260°C, respectively; times of extraction and desorption, 30 min and 5 min, respectively; ionic strength, 25% (w/v); rotate-speed, 600 rpm; solution pH, 5.0. Under the optimized conditions, limits of detection (S/N = 3) were 0.04 and 0.13 ng L(-1) for geosmin and 2-MIB, respectively. Calculated calibration curves gave high levels of linearity with a correlation coefficient value of 0.9999 for them. Finally, the proposed method was applied to water samples, which were previously analyzed and confirmed to be free of target analytes. Besides, the proposal method was applied to test environmental water samples. The RSDs were 2.75%~3.80% and 4.35%~7.6% for geosmin and 2-MIB, respectively, and the recoveries were 91%~107% and 91%~104% for geosmin and 2-MIB, respectively.

No MeSH data available.


Related in: MedlinePlus

To identify the two odors and the internal standard compound by HS-SPME.
© Copyright Policy - open-access
Related In: Results  -  Collection


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fig1: To identify the two odors and the internal standard compound by HS-SPME.

Mentions: To obtain the qualitative and quantitative ions, the two target analytes and the internal standard compound were first identified simultaneously by HS-SPME/GC-MS in the scan mode. The selected ions and retention time (tR) are listed in Table 2. The chromatogram (full-scan mode) is shown in Figure 1, and the full-scan mass spectra from 17.0 to 24.3 min were obtained with m/z range of 80–200 u.


Orthogonal Design Study on Factors Affecting the Determination of Common Odors in Water Samples by Headspace Solid-Phase Microextraction Coupled to GC/MS.

Peng S, Ding Z, Xia W, Zheng H, Xia Y, Chen X - J Anal Methods Chem (2013)

To identify the two odors and the internal standard compound by HS-SPME.
© Copyright Policy - open-access
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC3755388&req=5

fig1: To identify the two odors and the internal standard compound by HS-SPME.
Mentions: To obtain the qualitative and quantitative ions, the two target analytes and the internal standard compound were first identified simultaneously by HS-SPME/GC-MS in the scan mode. The selected ions and retention time (tR) are listed in Table 2. The chromatogram (full-scan mode) is shown in Figure 1, and the full-scan mass spectra from 17.0 to 24.3 min were obtained with m/z range of 80–200 u.

Bottom Line: The optimum was the following: temperatures of extraction and desorption, 65°C and 260°C, respectively; times of extraction and desorption, 30 min and 5 min, respectively; ionic strength, 25% (w/v); rotate-speed, 600 rpm; solution pH, 5.0.Calculated calibration curves gave high levels of linearity with a correlation coefficient value of 0.9999 for them.The RSDs were 2.75%~3.80% and 4.35%~7.6% for geosmin and 2-MIB, respectively, and the recoveries were 91%~107% and 91%~104% for geosmin and 2-MIB, respectively.

View Article: PubMed Central - PubMed

Affiliation: School of Public Health, Southeast University, Nanjing, Jiangsu 210009, China.

ABSTRACT
Geosmin and 2-MIB are responsible for the majority of earthy and musty events related to the drinking water. These two odorants have extremely low odor threshold concentrations at ng L(-1) level in the water, so a simple and sensitive method for the analysis of such trace levels was developed by headspace solid-phase microextraction coupled to gas chromatography/mass spectrometry. In this study, the orthogonal experiment design L32 (4(9)) was applied to arrange and optimize experimental conditions. The optimum was the following: temperatures of extraction and desorption, 65°C and 260°C, respectively; times of extraction and desorption, 30 min and 5 min, respectively; ionic strength, 25% (w/v); rotate-speed, 600 rpm; solution pH, 5.0. Under the optimized conditions, limits of detection (S/N = 3) were 0.04 and 0.13 ng L(-1) for geosmin and 2-MIB, respectively. Calculated calibration curves gave high levels of linearity with a correlation coefficient value of 0.9999 for them. Finally, the proposed method was applied to water samples, which were previously analyzed and confirmed to be free of target analytes. Besides, the proposal method was applied to test environmental water samples. The RSDs were 2.75%~3.80% and 4.35%~7.6% for geosmin and 2-MIB, respectively, and the recoveries were 91%~107% and 91%~104% for geosmin and 2-MIB, respectively.

No MeSH data available.


Related in: MedlinePlus