scholarly journals Multiresidue Method for Determination of Organochlorine Insecticides and Polychlorinated Biphenyl Congeners in Fatty Processed Foods

1996 ◽  
Vol 79 (6) ◽  
pp. 1434-1446 ◽  
Author(s):  
Anna Sannino ◽  
Paola Mambriani ◽  
Mirella Bandini ◽  
Luciana Bolzoni
Keyword(s):  
Polychlorinated Biphenyl ◽  
Methylene Chloride ◽  
Gas Chromatography Mass Spectrometry ◽  
Animal Origin ◽  
Electron Capture Detection ◽  
Matrix Interference ◽  
Selected Ion Monitoring ◽  
Pcb Congeners ◽  
Organochlorine Insecticides

Abstract A previously published gel permeation chromatographic (GPC) procedure for determination of organophosphorous insecticides is used to determine 24 organochlorine (OC) pesticide and 9 polychlorinated biphenyl (PCB) residues in 8 fatty preserved foods of vegetable and animal origin. Samples are extracted with methylene chloride and cleaned up by automated GPC with a Biobeads SX3 column and a methylene chloride–cyclohexane (15 + 85) eluant. Compounds are quantitated by gas chromatography/mass spectrometry (GC/MS) with selected ion monitoring using a DB-5 column. Average recoveries of OC pesticides from samples fortified at 0.010–0.080 mg/kg ranged from 73 to 98%. Average recoveries of 9 PCB congeners spiked at 2 levels (0.0025 and 0.020 mg/kg) were between 85 and 104%. Quantitation limits were between 0.002 and 0.025 mg/kg, depending on the compound. The purified extracts were analyzed further by GC with electron capture detection (ECD), and the results were compared with those obtained by MS. Determination of some OC pesticides and PCB congeners was not possible by ECD because of matrix interference.

Determination of Halogenated Contaminants in Human Adipose Tissue

1986 ◽  
Vol 69 (3) ◽  
pp. 451-458
Author(s):  
Guy L Lebel ◽  
David T Williams
Keyword(s):  
Gas Chromatography ◽  
Adipose Tissue ◽  
Methylene Chloride ◽  
Gel Permeation Chromatography ◽  
Human Adipose Tissue ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Fat Extraction ◽  
Capillary Column Gas Chromatography

Abstract <A method has been developed for determination of organochlorine contaminants in human adipose tissue. After fat extraction from the tissue with acetone-hexane (15 + 85, v/v), organochlorines were fractionated from fat by gel permeation chromatography with methylene chloride-cyclohexane (1 + 1, v/v) as solvent. After Florisil column cleanup, the GPC extract was analyzed by capillary column gas chromatography using 2 columns of different polarity. Compound identity was confirmed by gas chromatography-mass spectrometry using selected ion monitoring. Recoveries for fortification levels of 10-500 ng/g were greater than 80 % except for trichlorobenzene and hexachlorobutadiene (ca 60%).

Gas Chromatographic-Mass Spectrometric Determination of Six Sulfonamide Residues in Egg and Animal Tissues

1990 ◽  
Vol 73 (6) ◽  
pp. 886-892 ◽  
Author(s):  
Keigo Takatsuki ◽  
Tadashi Kikuchi
Keyword(s):  
Methylene Chloride ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Spectrometric Method ◽  
Mass Spectrometric Method ◽  
Animal Tissues ◽  
Selected Ion Monitoring ◽  
Ether Solution ◽  
Sulfonamide Residues

Abstract A gas chromatographlc-mass spectrometric method using selected Ion monitoring mode for simultaneous determination of 6 sulfonamides in egg and edible animal tissues has been developed. Sulfonamides are extracted from a sample with acetonltrlle. The extract Is passed through a silica cartridge column and concentrated. Dlazomethane in ether Is added to methylate sulfonamides. After evaporation, the residue Is dissolved In methylene chloride and cleaned up by silica gel column chromatography. The methylene chloride eluate containing sulfonamide-methyl derivatives Is evaporated to dryness, redlssolved In ether and partitioned between 6N hydrochloric acid. The acid phase is made alkaline, extracted with ether, and the ether solution, after concentration, Is analyzed by gas chromatography-mass spectrometry in selected Ion monitoring mode. Average recoveries from egg and silver salmon fortified at 1 and 0.2 ppm levels with 6 sulfonamides are 99.2 and 84.3%, respectively; coefficients of variation are 7.03 and 11.20%, respectively. Detection limits are 0.01-0.05 ppm.

scholarly journals Determination of N-Nitrosodimethylamine in Environmental Aqueous Samples by Isotope-Dilution GC/MS–SIM

2001 ◽  
Vol 84 (5) ◽  
pp. 1413-1419 ◽  
Author(s):  
Asit Raksit ◽  
Saima Johri
Keyword(s):  
Isotope Dilution ◽  
Anhydrous Sodium Sulfate ◽  
Methylene Chloride ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
Aqueous Samples ◽  
Method Detection Limit ◽  
Selected Ion Monitoring ◽  
Real Samples

Abstract An analytical method for the determination of N-nitrosodimethylamine (N-NDMA) in environmental aqueous samples has been developed using isotope dilution gas chromatography/mass spectrometry in the selected ion monitoring mode (GC/MS–SIM). After deuterated N-nitrosodimethylamine (d6-N-NDMA) as surrogate standard was added to the samples, the analytes were extracted with methylene chloride, dried with anhydrous sodium sulfate, and concentrated in a rotary evaporator. The concentrated extracts were analyzed by GC/MS–SIM after adding N-nitrosodiethylamine as an internal standard. The method detection limit for N-NDMA was 0.003 pg/μL and was validated by an analysis of a fortified water sample. The method was applied to real samples.

scholarly journals Application of Bar Adsorptive Microextraction for the Determination of Levels of Tricyclic Antidepressants in Urine Samples

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3101
Author(s):  
Mariana N. Oliveira ◽  
Oriana C. Gonçalves ◽  
Samir M. Ahmad ◽  
Jaderson K. Schneider ◽  
Laiza C. Krause ◽  
...  
Keyword(s):  
Tricyclic Antidepressants ◽  
Matrix Effects ◽  
Activated Carbons ◽  
Process Efficiency ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Experimental Conditions ◽  
Analytical Methodology ◽  
Low Efficiency

This work entailed the development, optimization, validation, and application of a novel analytical approach, using the bar adsorptive microextraction technique (BAμE), for the determination of the six most common tricyclic antidepressants (TCAs; amitriptyline, mianserin, trimipramine, imipramine, mirtazapine and dosulepin) in urine matrices. To achieve this goal, we employed, for the first time, new generation microextraction devices coated with convenient sorbent phases, polymers and novel activated carbons prepared from biomaterial waste, in combination with large-volume-injection gas chromatography-mass spectrometry operating in selected-ion monitoring mode (LVI-GC-MS(SIM)). Preliminary assays on sorbent coatings, showed that the polymeric phases present a much more effective performance, as the tested biosorbents exhibited low efficiency for application in microextraction techniques. By using BAμE coated with C18 polymer, under optimized experimental conditions, the detection limits achieved for the six TCAs ranged from 0.2 to 1.6 μg L−1 and, weighted linear regressions resulted in remarkable linearity (r2 > 0.9960) between 10.0 and 1000.0 μg L−1. The developed analytical methodology (BAμE(C18)/LVI-GC-MS(SIM)) provided suitable matrix effects (90.2–112.9%, RSD ≤ 13.9%), high recovery yields (92.3–111.5%, RSD ≤ 12.3%) and a remarkable overall process efficiency (ranging from 84.9% to 124.3%, RSD ≤ 13.9%). The developed and validated methodology was successfully applied for screening the six TCAs in real urine matrices. The proposed analytical methodology proved to be an eco-user-friendly approach to monitor trace levels of TCAs in complex urine matrices and an outstanding analytical alternative in comparison with other microextraction-based techniques.

Evidence of Organochlorine Pesticide and Polychlorinated Biphenyl Residues in Slovenian Poultry Tissues from 1997 to 1999

2004 ◽  
Vol 67 (10) ◽  
pp. 2326-2331 ◽  
Author(s):  
MOJCA JEVŠNIK ◽  
VESNA CERKVENIK FLAJS ◽  
DARINKA ZDENKA DOGANOC
Keyword(s):  
Public Health ◽  
Polychlorinated Biphenyl ◽  
Total Pcbs ◽  
Animal Origin ◽  
Fat Tissue ◽  
Public Health Perspective ◽  
Pcb Congeners ◽  
Poultry Fat ◽  
Tissue Contamination ◽  
Poultry Tissues

The contamination of poultry tissues by total organochlorine (OC) pesticides and polychlorinated biphenyls (PCBs) in Slovenia was examined from a public health perspective. As part of systematic veterinary and sanitary monitoring of foods of animal origin from 1997 to 1999, 87 samples of fat tissue were examined for the presence of α-HCH, lindane, heptachlor, and total DDT (plus DDE and DDD) and 88 samples of fat tissue were examined for the presence of total PCBs (sum of PCB congeners). The levels of poultry tissue contamination in six regions of Slovenia were determined. Levels of OC pesticides were below detection limits in 86.2% of analyses performed. Total PCB levels for most samples (59.1%) of poultry fat tissue were in the 0.002- to 0.02-mg/kg range. The level of contamination with OC pesticides and total PCBs in poultry fat tissue was not influenced by the type of poultry and was the highest in samples from industrial areas, which have been ecologically disturbed. All samples met Slovenian and European Union tolerances.

Simultaneous Determination of Alachlor, Metolachlor, Atrazine, and Simazine in Water and Soil by Isotope Dilution Gas Chromatography/Mass Spectrometry

1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.

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