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C ramped to 200
C at
30
Cmin
1
, then to 260
C at 3
Cmin
1
, and then to 320
C at
30
Cmin
1
heldfor 5min. One microliter of eachextract is injected
in split mode one twentieth using a Varian 8400 autosampler.
The injection port and transfer line temperatures are both xed at
300
-
dibromobiphenyle (ISTD) were purchased fromSigmaAldrich (St.
Quentin Fallavier, France), DPP (99.0% mixed of isomers), DiPP
(99.5%) and DnPP (99.0%) were obtained fromCIL Cluzeau Info Labo
(Sainte-Foy-La-Grande, France). Sodiumsulphate anhydrous came
from Panreac Quimica Sau (Barcelona, Spain). All organic solvents
(more than 99%) were obtained from different industrial sources
(VWR, Fluka, ChromaNorm).
Table 2
Analyzed phthalates.
Phthalates CAS number Legislation
DBP (dibutyl phthalate) 84-74-2 [A1,2,
3
] [B]
DEHP (diethylhexyl phthalate) 117-81-7 [A1,2,
3
] [B]
BBP (butylbenzyl phthalate) 85-68-7 [A1,2,
3
] [B]
DMEP (di(2-methoxyethyl) phthalate) 117-82-8 [A1,2,
3
]
DnPP (di-n-pentyl phthalate) 131-18-0 [A1,2,
3
]
DiPP (diisopentyl phthalate) 605-50-5 [A1,2,
3
]
DPP (n-pentyl isopentyl phthalate) 84777-06-0 [A1,2,
3
]
DiBP
a
(diisobutyl phthalate) 84-69-5 [A1,2,
3
] [B]
DCHP (dicyclohexyl phthalate) 84-61-7 [B]
DEP (diethyl phthalate) 84-66-2 [B]
DMP (dimethyl phthalate) 131-11-3 [B]
DnOP (di-n-octyl phthalate) 117-84-0 [B]
[A
1
] European regulation on cosmetics 1223/2009 30/11/2009 Annex-II (entrance
675, 677, 678, 1151 and 1152) and article 15.
[A
2
] European regulation 1272/2008 Annex VI.
[A
3
] European regulation 790/2009 Annexes II and V.
[B] Opinion on phthalates in cosmetic products. Scientic Committee on Consumer
Products (SCCP) 21/03/2007.
a
DiBP is regulated by the European cosmetic regulation 1223/2009 since the 1st
December 2010.
2.1.3. Standard solutions
The preparation and storage of standard solutions are per-
formed only with glass material to prevent the extraction of
phthalates fromplastics. The glassware is appropriately decontam-
inated before use [2,2022] by rinsing glassware several times with
an organic solvent (ethanol). During assay, ethyl acetate [23] is reg-
ularly injected to check and prevent carry over. Standard solutions
are prepared in ethanol by weighing 20.0mg of each phthalates
in a 20.0mL volumetric ask. These stock solutions can be used
for at least 7 days if they are stored in a refrigerator (see Section
3.2). A calibration curve ranging from 0.5gmL
1
to 5.0gmL
1
is prepared by diluting a 1000gmL
1
stock standard solution in
ethanol. 4,4
Cvs 77.1
C) leading
to an easier and faster evaporation of the extraction solvent during
the concentration step.
3.2. Preliminary validation criteria using the ISO 12787 standard
In agreement with the analytical approach described in the ISO
12787 standard, preliminary assay using standard solutions were
performed in order to check some general analytical elements like:
phthalates stability in solution, apparatus conformity (injection
repeatability, detector calibration, etc.). For phthalates, the detec-
tor calibration has been achieved via the performance of a mass
spectrometer auto-tune. The apparatus conformity was checked
by injecting 6 times a standard solution containing a mix of the 12
phthalates at 5.0gmL
1
. The RSDobtainedfor these solutions was
<3% for each phthalate considered in agreement with in-house
validationcriteria. In-house criteria were established fromdiffer-
ent documents in the eld of cosmetic and agro chemistry [3239].
An evaluation of phthalates stability in EtOH, by comparing ini-
tial solutions to fresh prepared solutions, was performed, results
pointed out an acceptable conservation of phthalates in stock solu-
tions for at least 7 days if stored in a refrigerator (absence of light
at approximately 4