کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
6551928 160421 2015 17 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Liquid chromatography with tandem mass spectrometry for the determination of flufenoxuron in blood using automatic solid phase extraction and its application to a fatal case of flufenoxuron poisoning
ترجمه فارسی عنوان
کروماتوگرافی مایع با اسپکترومتری جرمی دو طرفه برای تعیین فلوفنوکورون در خون با استفاده از استخراج فاز جامد و کاربرد آن در موارد کشنده مسمومیت با فلوفنکسورون
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
چکیده انگلیسی
A liquid chromatography/tandem mass spectrometry method with solid phase extraction for the detection and the quantitation of flufenoxuron in an aliquot of blood was developed and validated. Flufenoxuron belongs to a benzoylurea insecticide and is the active ingredient of Cascade™. The analyte in postmortem specimens was extracted by solid-phase extraction with Bond Elut Certify cartridge. After the elution layer was evaporated, the residue was reconstituted with 70% methanol for LC/MS/MS analysis. Separations were carried out on a Synergi® 2.5u Fusion-RP 100 A column with column temperature kept at 40 °C at a flow rate of 0.4 mL/min. The mobile phase was composed of 5 mM ammonium formate in 10% methanol and 5 mM ammonium formate in 90% methanol using gradient elution. A triple quadruple mass spectrometer equipped with an electrospray ionization source operated in a positive ion mode with selective reaction monitoring mode. Atrazine-d5 was used as internal standard. The assay was linear over 0.02-1.0 mg/L (r2 = 0.999). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were 0.009 mg/L (S/N = 3) and 0.02 mg/L (S/N = 10), respectively. The accuracy and the precision were <14.9% of bias% and <8.1% of CV%, which are acceptable criteria according to toxicology laboratory guidelines. Relative recoveries with 0.02, 0.1 and 1.0 mg/L (in blood) were 112.3%, 101.2% and 111.0% (n = 5), respectively. The developed method was applied in forensic toxicology to determine flufenoxuron in postmortem specimens in a fatal case of flufenoxuron intoxication in a 48-year-old-man who was found dead on bed in a small room after vomiting on the floor. The postmortem heart blood, peripheral blood and gastric contents were analyzed for flufenoxuron with the result of 6.3 mg/L in heart blood, 3.2 mg/L in peripheral blood and 30.6 mg/kg in gastric contents, respectively. The concentration ratio of the heart/peripheral blood of flufenoxuron was 2.0, and the ratio of gastric contents/peripheral blood was 9.4, suggesting possible postmortem redistribution and there may be a massive amount of flufenoxuron orally ingested. This case study is the first report of lethal concentrations of flufenoxuron in postmortem specimens.
ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Forensic Science International - Volume 257, December 2015, Pages 49-53
نویسندگان
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