Niquel em chocolate

2.4. Procedure for PV-IS-DLLME

The microextraction process was started with the addition of 5.0 mL of
the sample (or standard solution), with the pH adjusted to 2.0, to a test tube.
Then, 50.0 �L of a 0.10% (w/v) aqueous APDC solution and 120.0 �L of
([C4MIM][PF6]), were added. The mixture was aspirated with the aid of a glass
syringe. The syringe outlet was sealed, and the plunger was repeatedly moved
for 60 s. The plunger is pulled out and released quickly, causing a rapid
variation of pressure inside the syringe. At this time, the formation of the
emulsion occurred almost instantaneously through the pressure difference
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generated by the movement of the plunger. The plunger was always drawn to a
fixed point in the syringe (maximum of the scale), also fixing the number of
cycles. Afterwards, the mixture was transferred to a centrifuge tube, which was
centrifuged for 10 min at 3500 rpm in order to achieve phase separation. Then,
the supernatant was discarded and the enriched phase solubilized with 100 �L
of 10% (w/v) HNO3 in ethanol. The final blend was introduced into the flame
atomic absorption spectrometer to measure the nickel. Figure 1 shows a
schematic representation of this process.

Asadi
2.4 Microextraction procedure
The pH of 6.0 mL of the sample or standard solution was adjusted to 3.0 using
hydrochloric acid solution (1.0 mol L-1), the sample was placed in S1 and 110 �L of
1
dodecanol was added to it. Then, the S1 was connected to the S2. After that, the
mixture
injected into the S2 followed by back injection of the mixture in the S2 to the S1
(Figure S1).
At the end of extraction, the mixture was transferred into a centrifuge tube and
centrifuged at
5000 rpm for 5 min to separate the aqueous and organic phases. Then centrifuge tube
was
placed into an ice bath, and 1-dodecanol was solidified after 4 min. After that,
the solidified
www.jss-journal.com Page 6 Journal of Separation Science
1-dodecanol was collected and put in a conical vial where it melted immediately.
Finally, the
melted 1-dodecanol was injected into the HPLC for the determination of OTA.

Baby foods
Dispersive liquid-liquid microextraction
(DLLME): 60 �L of 1-octanol (extracting solvent)
and 600 �L of ethanol (disperser solvent) were
rapidly injected into the 10 mL sample solution, and
then 2 g of salt was added. The mixture was agitated
for two minutes. Thereafter, the cloudy solution was
centrifuged for 10 minutes at 4000 rpm. After this
process, a tiny droplet of 1-octanol was floated on the
aqueous sample. The lower-aqueous phase was
separated, and 20 �L of the floated phase was injected
directly into the HPLC using a Hamilton
microsyringe.

Sereshti
2.5. Procedure
1 mL of the sample solution was placed in a conical glass test
tube, and 0.1 g of sodium chloride added to it. Then, 200 lL of ethanol (dispersion
solvent) containing 20 lL of chloroform (extraction solvent) was injected into it
by using a syringe. Accordingly,
a cloudy solution (consisted of tiny droplets of chloroform dispersed in the
aqueous phase) was formed. In this step, extraction
of caffeine from aqueous phase into chloroform takes place. After
centrifugation of the cloudy solution at 4000 rpm for 2 min, the
extractant (chloroform) containing preconcentrated caffeine was
sedimented at the bottom of the test tube. Finally, 0.7 lL of the
sedimented organic phase was injected into GC�NPD. The performance and the
robustness of the procedure were examined with
lower volumes of sample solution. In this case, the procedure
was examined with 0.5 mL of sample solution and 100 lL of ethanol containing 10 lL
of chloroform with the salt concentration of
10%. The results confirm the possibility of performing the procedure for limited
volume samples. Although the procedure may be
performed directly on the undiluted samples, but the sample
pre-dilution may reduce the sample consumption and also simplifies the DLLME method
by reducing the matrix effect.

Shrivass
2.4. Procedure for DLLME for the determination of copper
109 A 13.0 mL of standard copper (5.0 ng/mL) aqueous solution was taken into
centrifugal
110 polyethylene tube with addition of 0.5 mL each of ascorbic acid, buffer
solution, 1.0% NaCl, 0.6
� 10-3
111 M DPT and total volume of the solution was 15.0 mL. Then, 0.5 mL absolute
ethanol
112 (dispersing solvent) and 0.2 mL of chloroform containing PBITU (extraction
solvent) were
113 injected into the aqueous phase and shaken for few minutes. The cloudy solution
was formed that
114 consisted of finely droplets of extraction solvent dispersed in the sample
solution. Finally, the
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115 centrifugation (REMI, R4C Centrifuge Machine) was carried out at 754.6 xg for 2
min, and the
116 organic phase at the top of the aqueous phase was carefully withdrawn using a
microsyringe and
117 placed into a tube. The obtained volume of the sample volume was found to be
small to analyze
118 in FAAS, so it was diluted to 400 �L with ethanol. This solution was directly
nebulised into the
119 flame without use of any particular injection system.