Simultaneous determination of phthalate di- and monoesters in poly(vinylchloride) products and human saliva by gas chromatography-mass spectrometry.
A gas chromatographic-mass spectrometric (GC-MS) method using selected ion monitoring (SIM) is described for the simultaneous determination of phthalate di- and monoesters in poly(vinylchloride) (PVC) products. The method consists of the following four procedures; (1). liquid-liquid extraction with ethyl acetate from the acidified aqueous homogenates of the PVC products, (2). esterification with trimethylsilyldiazomethane (TMSD) and methanol, (3). clean-up using Florisil column chromatography and (4). quantitative determination of methylated phthalate monoesters by GC-MS using SIM. The methylated monoesters show a characteristic mass fragment pattern at m/z 163, 149 and 91. The calibration curves for the monoesters were linear from 0.05 to 10 ng (injection volume 1 micro l). Overall recoveries ranged from 86.6 to 94.3%. The limits of detections for these methylated derivatives were in the range of 2.0-5.0 ng/g (S/N=3). This method was applied to phthalate monoesters in PVC toy products. Mono-n-butyl phthalate and mono-2-ethylhexyl phthalate were found at levels of 6.42-11.62 micro g/g and 30.50-41.81 micro g/g, respectively. No monoethyl phthalate, mono-n-hexyl phthalate and monobenzyl phthalate were found in the toy products. The method was also applied to these compounds in human saliva.
Niino
Tatsuhiro
T
Tokyo Kenbikyo-in Foundation, Center of Food and Environmental Sciences, 44-1 Nihonbashi Hakozaki-cho, Chuo-ku, Tokyo 103-0015, Japan. tatsu-n@jc4.so-net.ne.jp
Ishibashi
Tohru
T
Itho
Takeshi
T
Sakai
Senzo
S
Ishiwata
Hajimu
H
Yamada
Takashi
T
Onodera
Sukeo
S
D002138:Calibration; D004952:Esters; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D010795:Phthalic Acids / Q000032:analysis*; D011143:Polyvinyl Chloride / Q000032:analysis*; D012463:Saliva / Q000737:chemistry*; D012680:Sensitivity and Specificity
D004952:Esters; D010795:Phthalic Acids; C032279:phthalic acid; D011143:Polyvinyl Chloride