Experiment 7 : Analysis of Chlorpyrifos in Water by Solid-phase Extraction (SPE)

and Gas Chromatography-Electron Capture Detector (GC-ECD)

OBJECTIVE

To observe and record the analysis of chlorpyrifos in water by Solid-phase Extraction

(SPE) and Gas Chromatography-Electron Capture Detector (GC-ECD).

INTRODUCTION

Solid-phase extraction (SPE) is an extraction method that uses a solid phase and
a liquid phase to isolate one, or one type, of analyte from a solution. In other words, it is
a separation process by which compounds that are dissolved or suspended in a liquid
mixture are separated from other compounds in the mixture according to their physical
and chemical properties. Sorbents with different phases that commercially available
include non-polar (C8 and C18), polar (cyano and amino) and ion exchange sorbents.

Analytical laboratories use SPE to concentrate and purify samples for analysis.
Therefore, it is used in a wide variety of matrices, including urine, blood, water, beverages,
soil and animal tissue. The versatility of SPE allows it to be used for a number of
purposes, such as purification, trace enrichment, solvent exchange and derivatization.

SPE offers many benefits and advantages over more traditional sample
preparation techniques (liquid-liquid extraction) including high recoveries of analytes,
extraction reproducibility, reduction in organic solvent consumption and able to automate
the extraction process. SPE is used most often to prepare liquid samples and extract
semivolatile or nonvolatile analytes. Plus, it also can be used with solids that are pre-
extracted into solvents.

To separate a mixture into desired and undesired components, SPE uses the
affinity of solutes dissolved or suspended in a liquid that known as mobile phase for a
solid through which the sample is passed that known as stationary phase. The result is
either the desired analytes of interest or undesired impurities in the sample are retained
on the stationary phase. The portion that passes through the stationary phase is collected
or discarded but it is depends whether it contains the desired analytes or undesired
impurities. When the portion retained on the stationary phase includes the desired
analytes, they can then be removed from the stationary phase for collection in an
additional step in which the stationary phase is rinsed with an appropriate eluent.

For instrumentation, SPE use the same type of stationary phases as are used in
liquid chromatography column. The stationary phase is contained in a glass or plastic
column above a frit or glass wool. The column might have a frit on top of the stationary
phase and might also have a stopcock to control the flow of solvent through the column.
Commercial SPE catridges have 1 to 10mL capacities and are discarded after use.

Chlorpyrifos (O,O-diethyl O-3,5,6-trichloropyridin-2-yl phosphorothiote) is a

crystalline organophosphate insecticide. This broad-spectrum chlorpyrifos is one of the
top five residential pesticides in use for a wide variety of food crops, turf and ornamental,
and greenhouse. It acts on the nervous system of insects by inhibiting
acetylcholinesterase.

In addition, chlorpyrifos is no longer registered for use inside homes except as bait
in containers. This is because it is moderately toxic to humans and chronic exposure has
been linked to neurological effects, developmental disorders and autoimmune disorders.
But, it is still used in agriculture, on golf courses and to control public health pests such
as fire ants.

Chlorpyrifos blocks an enzyme that stops the nerve cells from firing without
stopping. If the enzyme is blocked, the nerves do not send normal signals and the nervous
system fails. It is moderately persistent in soils and is slightly soluble in water (2.0 mg L-
1). Plus, it has the potential to bioaccumulate.