Optimization and evaluation of low-pressure gas chromatography-mass spectrometry for the fast analysis of multiple pesticide residues in a food commodity.
ABSTRACT A fast method of analysis for 20 representative pesticides was developed using low-pressure gas chromatography-mass spectrometry (LP-GC-MS). No special techniques for injection or detection with a common quadrupole GC-MS instrument were required to use this approach. The LP-GC-MS approach used an analytical column of 10 m x 0.53 mm I.D., 1 microm film thickness coupled with a 3 m x 0.15 mm I.D. restriction capillary at the inlet end. Thus, the conditions at the injector were similar to conventional GC methods, but sub-atmospheric pressure conditions occurred throughout the analytical column (MS provided the vacuum source). Optimal LP-GC-MS conditions were determined which achieved the fastest separation with the highest signal/noise ratio in MS detection (selected ion monitoring mode). Due to faster flow-rate, thicker film, and low pressure in the analytical column, this distinctive approach provided several benefits in the analysis of the representative pesticides versus a conventional GC-MS method, which included: (i) threefold gain in the speed of chromatographic analysis; (ii) substantially increased injection volume capacity in toluene; (iii) heightened peaks with 2 s peak widths for normal MS operation; (iv) reduced thermal degradation of thermally labile analytes, such as carbamates; and (v) due to larger sample loadability lower detection limits for compounds not limited by matrix interferences. The optimized LP-GC-MS conditions were evaluated in ruggedness testing experiments involving repetitive analyses of the 20 diverse pesticides fortified in a representative food extract (carrot), and the results were compared with the conventional GC-MS approach. The matrix interferences for the quantitation ions were worse for a few pesticides (acephate, methiocarb, dimethoate, and thiabendazole) in LP-GC-MS, but similar or better results were achieved for the 16 other analytes, and sample throughput was more than doubled with the approach.
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ABSTRACT: Gas chromatography (GC) is used widely in applications involving food analysis. Typical applications pertain to the quantitative and/or qualitative analysis of food composition, natural products, food additives, flavor and aroma components, a variety of transformation products, and contaminants, such as pesticides, fumigants, environmental pollutants, natural toxins, veterinary drugs, and packaging materials. The aim of this article is to give a brief overview of the many uses of GC in food analysis in comparison to high-performance liquid chromatography (HPLC) and to mention state-of-the-art GC techniques used in the major applications. Past and current trends are assessed, and anticipated future trends in GC for food applications are predicted. Among the several new techniques being developed, the authors believe that, in food analysis applications, fast-GC/mass spectrometry (MS) will have the most impact in the next decade. Three approaches to fast-GC/MS include low-pressure GC/MS, GC/time-of-flight (TOF)-MS and GC/supersonic molecular beam (SMB)-MS, which are briefly discussed, and their features are compared.TrAC Trends in Analytical Chemistry 09/2002; 21(s 9–10):686–697. · 6.61 Impact Factor
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ABSTRACT: Emerging flame retardants are used in a great variety of household goods and thus have the potential to pollute our indoor environment. Health concerns regarding exposure to these flame retardants demand new methods to survey their occurrence in humans. This work describes development and optimization of an analytical method comprising solid phase extraction and gas chromatography coupled to mass spectrometry for the determination of besides 15 polybrominated diphenyl ethers, 7 emerging halogenated flame retardants in human serum (1,2-bis[2,4,6-tribromophenoxy] ethane, decabromodiphenyl ethane, hexabromobenzene, Dechlorane Plus(®), hexachlorocyclopentenyl-dibromocyclooctane, dechlorane 602 and 603). The method was thoroughly validated at three spiking levels obtaining averaged recoveries >80% with a RSD of 5% (n=12). Accuracies ranged from 88 to 125% except for DBDPE, which averaged 66% with overall RSD of 11% (n=12). Method limits of detection (MLD) ranged from 0.3 to 5.4pg/mL serum, except for decabromodiphenyl ether and decabromodiphenyl ethane for which MLDs were 14 and 20pg/mL serum, respectively. In human serum samples from Norway, we were able to detect and quantify hexabromobenzene, 1,2-bis[2,4,6-tribromophenoxy] ethane, Dechlorane Plus(®), Dechlorane 602 and 603.Journal of Chromatography A 08/2013; · 4.61 Impact Factor
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ABSTRACT: An alternative to conventional capillary gas chromatography (GC) is evaluated as a new approach to determine pesticide residues in vegetables. Low-pressure gas chromatography–tandem mass spectrometry (LP-GC–MS–MS) is proposed after a fast and simple extraction of the vegetable samples with dichloromethane and without clean up. The use of the above-mentioned GC technique reduced the total time required to determine 72 pesticides to less than half the present time (31 min), increasing the capability of a monitoring routine laboratory. The use of guard column and plug of carbofrit into the glass liner in combination with LP-GC was evaluated. The method was validated with limits of quantitation low enough to determine the pesticide residues at concentrations below the maximum residue levels stated by legislation. In order to assess its applicability to the analysis of real samples, 25 vegetable samples previously determined using conventional-capillary GC–MS–MS were analysed by LP-GC–MS–MS. The results obtained with the compared techniques showed differences lower than 0.01 mg kg−1.Journal of Chromatography A - J CHROMATOGR A. 01/2003; 1005(1):131-141.
EASTERN REGIONAL RESEARCH CENTER
AGRICULTURAL RESEARCH SERVICE
UNITED STATES DEPARTMENT OF AGRICULTURE
600 E. MERMAID LANE
WYNDMOOR, PA 19038
Optimization and Evaluation of Low-Pressure Gas Chromatography-Mass
Spectrometry for the Fast Analysis of Multiple Pesticide Residues in a Food
Author(s): K. Mastovska, S.J. Lehotay and J. Hajslova
Journal of Chromatography A (2001) 926: 291-308
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