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Analysis of phthalic acid esters in biological
samples
[Outline]
Phthalic acid esters (PAEs)1,2, extracted from biological
samples with acetonitrile and purified by Florisil-PSA column
chromatography, are analyzed by a gas chromatograph/mass
spectrometer (GC/MS) qualitatively and quantitatively.
The esters analyzed here are dibutyl phthalate (DBP),
butylbenzyl phthalate (BBP), di-2-ethylhexyl phthalate (DEHP),
diisooctyl phthalate (DiOP) and diisononyl phthalate (DiNP).
This method can be applied to serum.
[Reagents]
Confirm by chromatography that all the reagents present no
problem in PAE analysis.
(i) Organic solvents: n-Hexane, acetonitrile and acetone of PAE
analysis grade. Open the seal immediately before use3.
(ii) Anhydrous odium sulfate: Residual pesticide analysis grade;
heat to 200 for 2 hours and let cool down before use.
(iii) Sodium chloride: PAE analysis grade; heat to 200 for 2
hours and let cool down before use.
(iv) Purified water: Distilled water after washing with n-hexane
of the PAE analysis grade4.
(v) Florisil: Florisil PR; heat to 200 for 2 hours and let cool
down before use.
(vi) PSA: Bondesil PSA.
(vii) Standard PAE solutions: Place 20 mg each of standard
products in 20 ml measuring flasks and add n-hexane to 20 ml to
obtain 1000Ęg/ml solutions. Dilute as appropriate.
(viii) Internal standards: Place 20 mg each of standard PAE-d4
in 20 ml measuring flasks and add n-hexane to 20 ml to obtain
1000Ęg/ml solutions. Dilute as appropriate.
[Apparatus]
(i) Gas chromatograph/mass spectrometer (GC/MS): A unit capable
of selective ion monitoring (SIM) equipped with an ion source by
electron ionization and a capillary column (splitless)
(ii) Florisil-PSA column: Fill a glass chromatographic column,
15 mm i.d. and 110 mm long, with 1 g Florisil and 0.5 g PSA and
2 g anhydrous sodium sulfate upon it. Wash the column with 10 ml
acetone and 10 ml n-hexane before use.
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