Cooling a 1:1 (v/v) solution of acetonitrile and water at
−16° C is known to result in two clear phases. We will refer to
this event as “cold-induced aqueous acetonitrile phase separation
(CIPS)”. On a molar basis, acetonitrile is 71.7% and
13.6% in the upper and lower phases, respectively, in our study. The
phase separation proceeds as a descending cloud of microdroplets. At the
convenient temperature (typical freezer) employed here the lower phase is rather
resistant to solidification, although it emerges from the freezer as a solid if
various insoluble matter is present at the outset. In a preliminary way, we
replaced the initial (salting-out) step of a representative QuEChERS procedure
with CIPS, applying this modified procedure (“CIPS-QuEChERS”) to
a homogenate of salmon (and partly to beef). Three phases resulted, where only
the upper, acetonitrile-rich phase is a liquid (that is completely clear). The
middle phase comprises ice and precipitated lipids, while the lower phase is the
residual matrix of undissolved salmon or meat. Treating the upper phase from
salmon, after isolation, with anhydrous MgSO4 and C18-Si (typical
QuEChERS dispersive solid phase extraction sorbents), and injecting into a
GC–MS in a nontargeted mode, gives two-fold more preliminary hits for
chemicals, and also number of spiked pesticides recovered, relative to that from
a comparable QuEChERS method. In part, this is because of much higher background
signals in the latter case. Further study of CIPS-QuEChERS is encouraged,
including taking advantage of other QuERChERS conditions.