scholarly journals Development of a Solid Phase Extraction-based Method for Quantitative Analysis of Methylmercury in Soil and Sediment

2021 ◽  
Author(s):  
Sachiko Kakimoto ◽  
Masato Yoshimitsu ◽  
Kyohei Kiyota
Keyword(s):  
Solid Phase Extraction ◽  
Paddy Soil ◽  
Solid Phase ◽  
Health Hazard ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Universal Method ◽  
Soil Matrix ◽  
Reference Samples ◽  
Soil And Sediment

Abstract Methylmercury (MeHg) pollution is currently widespread in paddy soil and sediment, posing a health hazard risk during the harvesting of rice grains. However, to date, a simple and universal method for quantifying MeHg in the soil is unavailable. Therefore, we aimed to develop a solid-phase extraction-based method using gas chromatography mass spectrometry (GC-MS). In this study, MeHg was purified from the soil matrix using optimized solid-phase extraction; our method reduced the use of organic solvents and did not require harmful reagents such as alkaline solution and toluene. The limit of quantification in the sample was determined to be 7.5 ng/g. The MeHg recovery in reference samples was 96.2–102.6%, and intra- and inter-assay coefficients of variation were 3.4–7.1% and 4.3–7.1%, respectively, indicating high validation performance. Furthermore, the MeHg levels of the five tested reference samples were determined to be 64.1 ng/g or not detected, and these levels were well below the Japanese regulatory criteria. This new method could provide reliable and useful data for environmentalists and agriculturalists to prevent MeHg pollution, facilitating the improvement of food safety for harvests from paddy soil.

scholarly journals A high-throughput and sensitive methodology for the quantification of urinary 8-hydroxy-2′-deoxyguanosine: measurement with gas chromatography-mass spectrometry after single solid-phase extraction

2004 ◽  
Vol 380 (2) ◽  
pp. 541-548 ◽  
Author(s):  
Hai-Shu LIN ◽  
Andrew M. JENNER ◽  
Choon Nam ONG ◽  
Shan Hong HUANG ◽  
Matthew WHITEMAN ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Healthy Subjects ◽  
Solid Phase ◽  
Large Population ◽  
Urine Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Freeze Dried ◽  
Wide Range

8-Hydroxy-2´-deoxyguanosine (8OHdG) is a widely used biomarker for the measurement of endogenous oxidative DNA damage. A sensitive method for the quantification of 8OHdG in urine by single solid-phase extraction and GC-MS (gas chromatography with MS detection) using selective ion monitoring is described in the present study. After solid-phase extraction, samples are freeze-dried, derivatized by trimethylsilylation and analysed by GC-MS. The urinary 8OHdG was quantified using heavy isotope dilution with [18O]8OHdG. The recovery of 8OHdG after the solid-phase extraction ranged from 70 to 80% for a wide range of urinary 8OHdG levels. Using 1 ml of urine, the limit of quantification was >2.5 nM (2.5 pmol/ml) and the calibration curve was linear in the range 2.5–200 nM. This method was applied to measure 8OHdG in urine samples from 12 healthy subjects. The intra- and inter-day variations were <9%. Urinary 8OHdG levels in spot urine samples from four healthy subjects were also measured for 1 week and, again, the variation was small. The presence of H2O2 in urine did not cause artifactual formation of 8OHdG. Since this assay is simple, rapid, sensitive and reproducible, it seems suitable to be used as a routine methodology for the measurement of urinary excretion of 8OHdG in large population studies.

Sign in / Sign up

Export Citation Format

Share Document