title: Gas purge microsyringe extraction for quantitative direct gas chromatographic-mass spectrometric analysis of volatile and semivolatile chemicals.
abstract: Sample pretreatment before chromatographic analysis is the most time consuming and error prone part of analytical procedures, yet it is a key factor in the final success of the analysis. A quantitative and fast liquid phase microextraction technique termed as gas purge microsyringe extraction (GP-MSE) has been developed for simultaneous direct gas chromatography-mass spectrometry (GC-MS) analysis of volatile and semivolatile chemicals without cleanup process. Use of a gas flowing system, temperature control and a conventional microsyringe greatly increased the surface area of the liquid phase micro solvent, and led to quantitative recoveries of both volatile and semivolatile chemicals within short extraction time of only 2 min. Recoveries of polycyclic aromatic hydrocarbons (PAHs), organochlorine pesticides (OCPs) and alkylphenols (APs) determined were 85-107%, and reproducibility was between 2.8% and 8.5%. In particular, the technique shows high sensitivity for semivolatile chemicals which is difficult to achieve in other sample pretreatment techniques such as headspace-liquid phase microextraction. The variables affecting extraction efficiency such as gas flow rate, extraction time, extracting solvent type, temperature of sample and extracting solvent were investigated. Finally, the technique was evaluated to determine PAHs, APs and OCPs from plant and soil samples. The experimental results demonstrated that the technique is economic, sensitive to both volatile and semivolatile chemicals, is fast, simple to operate, and allows quantitative extraction. On-site monitoring of volatile and semivolatile chemicals is now possible using this technique due to the simplification and speed of sample treatment.
authors.affiliation: Key Laboratory of Nature Resource of the Changbai Mountain and Functional Molecular, Yanbian University, Ministry of Education, Park Road 977, Yanji City, Jilin Province 133002, China.
authors.forename: Cui
authors.initials: C
authors.lastname: Yang
authors.forename: Xiangfan
authors.initials: X
authors.lastname: Piao
authors.forename: Jinxue
authors.initials: J
authors.lastname: Qiu
authors.forename: Xiaoping
authors.initials: X
authors.lastname: Wang
authors.forename: Chunyan
authors.initials: C
authors.lastname: Ren
authors.forename: Donghao
authors.initials: D
authors.lastname: Li
mesh_terms: D005591:Chemical Fractionation / Q000295:instrumentation / Q000379:methods*; D002851:Chromatography, High Pressure Liquid; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006586:Hexanes; D006843:Hydrocarbons, Chlorinated / Q000032:analysis* / Q000302:isolation & purification; D010575:Pesticides / Q000032:analysis / Q000302:isolation & purification; D010636:Phenols / Q000032:analysis / Q000302:isolation & purification; D010944:Plants / Q000737:chemistry; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis* / Q000302:isolation & purification; D012987:Soil / Q000737:chemistry; D013696:Temperature; D055549:Volatile Organic Compounds / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D006586:Hexanes; D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; D010636:Phenols; D011084:Polycyclic Aromatic Hydrocarbons; D012987:Soil; D055549:Volatile Organic Compounds