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J Chromatogr A ; 1603: 61-66, 2019 Oct 11.
Article in English | MEDLINE | ID: mdl-31262514

ABSTRACT

A simple procedure based on microextraction by packed sorbent (MEPS) has been proposed for the extraction of dichloropane in oral fluids and its determination by ion mobility spectrometry (IMS). Extraction conditions such as type of sorbent (octyl and octadecyl silica), sample pH, number of sample loadings, and elution volume were evaluated to obtain the most appropriate values. Dichloropane was extracted from saliva samples using C8 MEPS, loading with 100 µL sample (adjusted to pH 7) in 4 cycles, washing with 100 µL deionized water, and eluting with 50 µL 2-propanol in 10 cycles. The proposed MEPS procedure has been validated in terms of linearity, accuracy, and precision. A limit of detection of 30 µg L-1 was obtained for dichloropane determination in saliva. The analysis of field and synthetic saliva samples spiked with dichloropane at concentration levels from 250 to 750 µg L-1 provided relative recoveries between 85 and 110%, using the proposed MEPS-IMS procedure. Field oral fluid samples were collected from healthy individuals, blind-spiked from 92 to 278 µg L-1, and analysed by IMS and gas chromatography-mass spectrometry, being the results obtained from both methods statistically comparable. Thus, the proposed MEPS-IMS procedure involves a simple, sensitive, and accurate analysis of dichloropane in saliva.


Subject(s)
Cocaine/analogs & derivatives , Gas Chromatography-Mass Spectrometry/methods , Ion Mobility Spectrometry/methods , Saliva/chemistry , Solid Phase Microextraction/methods , Cocaine/analysis , Humans , Limit of Detection
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