Biomaterial Database

Development and interlaboratory validation of a QuEChERS-based liquid chromatography-tandem mass spectrometry method for multiresidue pesticide analysis. 2010

Jon Wong, and Chunyan Hao, and Kai Zhang, and Paul Yang, and Kaushik Banerjee, and Douglas Hayward, and Imran Iftakhar, and Andre Schreiber, and Katherine Tech, and Chris Sack, and Michael Smoker, and Xiangru Chen, and Sagar C Utture, and Dasharath P Oulkar

Center for Food Safety and Applied Nutrition, US Food and Drug Administration, College Park, Maryland 20740-3835, USA.

A high-throughput, QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) sample preparation and liquid chromatography-tandem mass spectrometry (LC-MS/MS) analytical method has been developed and validated for the determination of 191 pesticides in vegetation and fruit samples. Using identical LC analytical column and MS/MS instrumentation and operation parameters, this method was evaluated at the U.S. Food and Drug Administration (FDA), National Research Centre for Grapes (NRCG), India, and Ontario Ministry of the Environment (MOE) laboratories. Method validation results showed that all but 1 of these 191 pesticides can be analyzed by LC-MS/MS with instrument detection limits (IDL) in the parts per trillion (ppt) range. Matrix-dependent IDL studies showed that due to either the low ionization efficiency or matrix effect exerted, 14 of these 191 pesticides could not be analyzed by this method. Method recovery (%R) and method detection limits (MDLs) were determined by the three laboratories using four sample matrices in replicates (N = 4). With >79% of %R data from the fortification studies in the range from 80 to 120%, MDLs were determined in the low parts per billion range with >94% of MDLs in the range from 0.5 to 5 ppb. Applying this method to the analysis of incurred samples showed that two multiple reaction monitoring (MRM) transitions may not be enough to provide 100% true positive identification of target pesticides; however, quantitative results obtained from the three laboratories had an excellent match with only a few discrepancies in the low parts per billion levels. The %R data from the fortification studies were subjected to principal component analysis and showed the majority of %R fell into the cluster of 80% < %R < 120%. Due to the matrix effect exerted by ginseng and peach, outliers were observed at the lowest spiking levels of 10 and 25 ppb. The study also showed that QuEChERS samples should be analyzed as soon as prepared or stored in a freezer to avoid any adverse affect on the analytes evaluated.

UI	MeSH Term	Description	Entries
D007753	Laboratories	Facilities equipped to carry out investigative procedures.	Laboratory
D010573	Pesticide Residues	Pesticides or their breakdown products remaining in the environment following their normal use or accidental contamination.	Pesticide Residue,Residue, Pesticide,Residues, Pesticide
D010936	Plant Extracts	Concentrated pharmaceutical preparations of plants obtained by removing active constituents with a suitable solvent, which is evaporated away, and adjusting the residue to a prescribed standard.	Herbal Medicines,Plant Extract,Extract, Plant,Extracts, Plant,Medicines, Herbal
D011786	Quality Control	A system for verifying and maintaining a desired level of quality in a product or process by careful planning, use of proper equipment, continued inspection, and corrective action as required. (Random House Unabridged Dictionary, 2d ed)	Control, Quality,Controls, Quality,Quality Controls
D002853	Chromatography, Liquid	Chromatographic techniques in which the mobile phase is a liquid.	Liquid Chromatography
D005591	Chemical Fractionation	Separation of a mixture in successive stages, each stage removing from the mixture some proportion of one of the substances, for example by differential solubility in water-solvent mixtures. (McGraw-Hill Dictionary of Scientific and Technical Terms, 4th ed)	Fractionation, Chemical,Chemical Fractionations,Fractionations, Chemical
D005638	Fruit	The fleshy or dry ripened ovary of a plant, enclosing the seed or seeds.	Berries,Legume Pod,Plant Aril,Plant Capsule,Aril, Plant,Arils, Plant,Berry,Capsule, Plant,Capsules, Plant,Fruits,Legume Pods,Plant Arils,Plant Capsules,Pod, Legume,Pods, Legume
D005894	Panax	An araliaceous genus of plants that contains a number of pharmacologically active agents used as stimulants, sedatives, and tonics, especially in traditional medicine. Sometimes confused with Siberian ginseng (ELEUTHEROCOCCUS).	Ginseng,Korean Ginseng,Korean Red Ginseng,Panax ginseng,Jen Shen,Ninjin,Renshen,Schinseng,Shinseng,Ginseng, Korean,Ginseng, Korean Red,Ginsengs,Jen Shens,Korean Ginsengs,Korean Red Ginsengs,Ninjins,Red Ginseng, Korean,Renshens,Schinsengs,Shen, Jen,Shinsengs
D014675	Vegetables	A food group comprised of EDIBLE PLANTS or their parts.	Vegetable
D053719	Tandem Mass Spectrometry	A mass spectrometry technique using two (MS/MS) or more mass analyzers. With two in tandem, the precursor ions are mass-selected by a first mass analyzer, and focused into a collision region where they are then fragmented into product ions which are then characterized by a second mass analyzer. A variety of techniques are used to separate the compounds, ionize them, and introduce them to the first mass analyzer. For example, for in GC-MS/MS, GAS CHROMATOGRAPHY-MASS SPECTROMETRY is involved in separating relatively small compounds by GAS CHROMATOGRAPHY prior to injecting them into an ionization chamber for the mass selection.	Mass Spectrometry-Mass Spectrometry,Mass Spectrometry Mass Spectrometry,Mass Spectrometry, Tandem