Analyses of lindane, vinclozolin, aldrin, p,p′-DDE, o,p′-DDT and p,p′-DDT in human serum using gas chromatography with electron capture detection and tandem mass spectrometry

Author(s):  
M Moreno Frı́as ◽  
A Garrido Frenich ◽  
J.L Martı́nez Vidal ◽  
M Mateu Sánchez ◽  
F Olea ◽  
...  
1990 ◽  
Vol 73 (4) ◽  
pp. 529-533 ◽  
Author(s):  
Jean E Matusik ◽  
Richard S Sternal ◽  
Charlie J Barnes ◽  
James A Sphon

Abstract Four sulfonamide veterinary drug residues were quantltated by electron-capture detection (ECD) after separation by gas chromatography (GC). The Identities of sulfathiazole (ST), sulfamethazine (SM), sulfachloropyridazine (SCP), and sulfadimethoxine (SDM) were confirmed In bovine or swine liver residues by tandem mass spectrometry (MS/MS). Bovine or swine liver tissues were extracted by using either the Tlshler or the Manuel-Steller cleanup. The methylated residues containing ST, SM, SCP, and SDM were separated by GC prior to MS/MS daughter ion analysis. Control tissue, control tissue fortified at 0.1 ppm, and Incurred tissue residues at approximately 0.1 ppm were analyzed for these 4 sulfonamides. A Flnnigan Model TSQ-46 operating in the chemical ionization mode was used to perform the MS/MS daughter Ion experiments. The Identities of all 4 sulfonamides were confirmed In a single GC/MS/MS analysis.


2001 ◽  
Vol 84 (6) ◽  
pp. 1751-1762 ◽  
Author(s):  
Antonia Garrido Frenich ◽  
Maria Del Carmen Pablos Espada ◽  
Jose Luis Martínez Vidal ◽  
Luis Molina

Abstract Gas chromatography with electron capture detector (ECD), nitrogen–phosphorus detector (NPD), and tandem mass spectrometry (MS/MS) was used to identify 36 pesticides, widely used to control various pest and diseases in vegetables, in water after a preconcentration step on C18 cartridges. The recoveries obtained ranged from 70 to 135% at a fortification level of 100 ng/L with relative standard deviations of <36.2%. The limits of detection and quantitation were ≤48 and ≤160 ng/L, respectively. Important advantages of MS/MS over ECD and NPD in the determination of pesticides are also presented. The proposed analytical methodology was applied to the determination of pesticides in groundwater samples from an agricultural area, the Campo de Dalías (Almería, Spain). The most frequently encountered pesticides were endosulfan sulfate and metalaxyl, whereas the pesticide found at the highest concentration was fenamiphos.


2020 ◽  
Vol 103 (6) ◽  
pp. 1461-1468
Author(s):  
Guru Prasad Katuri ◽  
Xinghua Fan ◽  
Shabana Siddique ◽  
Cariton Kubwabo ◽  
Ivana Kosarac ◽  
...  

Abstract Background Synthetic musk compounds are widely used as fragrances in many consumer products; however, information on human exposure and health effects is limited. Also, analytical methods for their quantification in biological matrices are limited. Objective In this study, an integrated method was developed and validated for the analysis of selected synthetic musk compounds in human serum. Method The method is based on liquid-liquid extraction (LLE), sample clean-up by solid-phase extraction (SPE), and separation and detection by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). Results The method demonstrated good recoveries (86–105%) and high sensitivity, with low method detection limits (MDLs) ranging from 0.04 to 0.17 µg/L. The method was applied to the analysis of 10 synthetic musk compounds in 40 serum samples collected from Canadian women aged 20–44 years (20 individual samples collected in 2014 and 20 pooled samples collected in 2006). The most commonly detected compound was Galaxolide (HHCB), with median concentrations of 0.59 µg/L in samples collected in 2006, and 0.34 µg/L for samples collected in 2014. Musk ketone (MK) was not detected in any of the samples collected in 2006, but was detected in 60% of the samples collected in 2014 with a median concentration of 0.29 µg/L. Tonalide (AHTN) was detected in only one sample above its MDL (0.12 µg/L). Conclusions This is the first study in Canada to report levels of synthetic musks in human. The data generated from this study has been used in risk screening assessment by Environment and Climate Change Canada and Health Canada.


Sign in / Sign up

Export Citation Format

Share Document