Simultaneous determination of phthalate di- and monoesters in poly(vinylchloride) products and human saliva by gas chromatography–mass spectrometry

Niino, Tatsuhiro; Ishibashi, Tohru; Itho, Takeshi; Sakai, Senzo; Ishiwata, Hajimu; Yamada, Takashi; Onodera, Sukeo

doi:10.1016/s1570-0232(02)00413-0

Cited by 35 publications

(31 citation statements)

References 20 publications

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“…Instruments ---GC/MS analysis was performed by the method described in the previous paper. 10) HPLC operating conditions required to detect phthalic acid and phthalate monoesters were as follows: apparatus, LC-10A (Shimadzu, Kyoto, Japan); column, Inertsil C8-3 (0.46 mm φ × 250 mm); column oven temperature, 40°C; mobile phase, 0.1% acetic acid including 5.0 mmol/l tetra-n-butylammonium phosphate solution/acetonitrile (50 : 50); detector, UV (254 nm); and injection volume, 10 µl.…”

Section: Introductionmentioning

confidence: 99%

Characterization of Human Salivary Esterase in Enzymatic Hydrolysis of Phthalate Esters.

Niino

Ishibashi

Ishiwata³

et al. 2003

JOURNAL OF HEALTH SCIENCE

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tyl phthalate (DBP). 1)Some phthalate diesters induce testicular toxicity in the male reproductive tract. Jobling et al. showed that DBP binds to the estrogen receptor, displaces its natural ligand, and then acts as an estrogen antagonist.2) In addition, mono-n-butyl phthalate (MBuP) adversely affects development of the reproductive system in male rats.3) DEHP is a peroxisome proliferator that induces tumors in the rodent liver, and this effect is probably not exerted by DEHP itself but by one or more of its metabolites. 4)Phthalate diesters are metabolized to monoesters by hydrolases in many tissues, such as the pancreas, intestine, and blood.5-7) Generally orally ingested dialkyl phthalates are hydrolyzed by esterases in the wall of the small intestine and pancreatic lipases and not by gut flora. Absorption occurs almost entirely as the corresponding monoesters.5) Human saliva is a matrix of inorganic compounds, saliva proteins such as lingual lipase and α-amylase, oral flora, and cell debris. 8) However, to the best of our knowledge there are no reports concerning enzymatic hydrolysis of phthalate diesters in human saliva, except for our previous paper.9) The present work was therefore designed to characterize human salivary esterase in enzymatic hydrolysis of phthalate esters. These findings provide the information that will be required in considering the human health effects of phthalate esters. MATERIALS AND METHODSChemicals and Glassware ---Monoethyl phthalate (MEP), diethyl phthalate (DEP), and DEHP were purchased from Wako Pure Chemical Industries. (Osaka, Japan) and MBuP, mono-n-hexyl phthalate (MHxP), mono-2-ethylhexyl phthalate (MEHP), monobenzyl phthalate (MBeP), and di-n-hexyl phEnzymatic hydrolysis of phthalate esters in human saliva was investigated to characterize salivary esterase in the formation of monoesters from their diesters. The monoesters formed were analyzed by GC/ MS after incubation of phthalate diesters in the saliva. Hydrolytic activity in the supernatant obtained by centrifugation of the saliva at 1350 × g was equivalent to that in whole saliva, and the activity was inhibited by the addition of denaturing protein. The hydrolytic activity was dependent on the protein concentration in the supernatant. The optimum temperature and pH of the hydrolysis was 50°C and 8.2, respectively. In addition, the 80% acetone powder of the supernatant showed high substrate specificity for straight-chain alkyl group of phthalate diesters, especially the butyl group, whereas almost no specificity was seen for the 2-ethylhexyl and benzyl groups. These results indicate that not the oral flora but salivary esterase, such as lingual lipase, is involved in phthalate monoester formation from the diesters in human saliva, and do not act on the hydrolysis of monoester.

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Section: Introductionmentioning

confidence: 99%

Characterization of Human Salivary Esterase in Enzymatic Hydrolysis of Phthalate Esters.

Niino

Ishibashi

Ishiwata³

et al. 2003

JOURNAL OF HEALTH SCIENCE

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“…In recent years, several methods for the determination of phthalates by gas chromatography (GC) [1,[5][6][7][8][9][10] and by high performance liquid chromatography (HPLC) [11][12][13][14][15][16][17][18][19][20] were described. Different methods of sample preparation and extraction have been used, such as liquid -liquid extraction (LLE) [7,21] , solid phase extraction (SPE) [1,6,11,12,16,17,21] , solid phase microextraction (SPME) [8,20,22,23] , supercritical fluid extraction [21] , microwave extraction [13,21] , Soxhlet extraction [10,21,24] and ultrasonic extraction [5,21,25] . In this paper, the studies of gas chromatography in combination with mass spectrometry detector (MS) and electron capture detector (ECD) for determination of seven kinds of phthalates, e.g.…”

Section: Introductionmentioning

confidence: 99%

Determination of Phthalates in Polymer Materials Comparison of GC/MS and GC/ECD methods

Jaworek¹,

Czaplicka²

2013

Polímeros

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The paper presents two methods for determination of phthalates in polymer materials. The methods compared were gas chromatography combined with the mass spectrometry (GC/MS) and gas chromatography with electron capture detector (GC/ECD). The GC/ECD technique was chosen for this comparison, because the ECD detector was one of few capable of detecting phthalates. In both cases the same procedure of sample preparation with ultrasonic extraction was applied. Overall recoveries were 76-100 % with relative of standard deviation (R.S.D.) values in the range 0.6-19 %. The values of limit of detection (LOD) for GC/MS method ranged from 3.46 µg mL -1 to 10.10 µg mL -1 , depending on the determined phthalate, while in case of the GC/ECD method they were in the range from 2.97 µg mL -1 to 4.29 µg mL -1 . The methods were applied for determination of: dimethyl phthalate, diethyl phthalate, di-n-butyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl) phthalate, diisononyl phthalate, diisoocyl phthalate in polymer material. The seventeen kinds of samples were analyzed. Most of the materials selected for the analyses were made from polyethylene (PE), polyvinyl chloride (PVC) and polystyrene (PS).

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“…The extracts are usually analyzed using chromatographic or spectroscopic methods. 4 Solvent-based sample preparation, however, is time consuming, requires extensive clean-up of the glassware and large volumes of solvents, and often causes poorer data quality due to multiple sample preparation steps. Now, these circumstances strongly request the development of rapid and simple determination methods of phthalates in plastic samples.…”

Section: Introductionmentioning

confidence: 99%

Rapid and Simple Determination of Phthalates in Plastic Toys by a Thermal Desorption-GC/MS Method

Yuzawa¹,

Watanabe²,

Freeman

et al. 2009

ANAL. SCI.

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A thermal desorption (TD)-GC/MS method was applied for the determination of phthalates in plastic children's toys. The method, which does not need any cumbersome sample pretreatment such as solvent extraction, filtration and derivatization, has been proved to be useful not only as a sensitive analytical method to evaluate phthalate concentration in the toys, but also as a rapid and practical screening method to check whether the concentration exceeds the regulatory limit.

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Simultaneous determination of phthalate di- and monoesters in poly(vinylchloride) products and human saliva by gas chromatography–mass spectrometry

Cited by 35 publications

References 20 publications

Characterization of Human Salivary Esterase in Enzymatic Hydrolysis of Phthalate Esters.

Characterization of Human Salivary Esterase in Enzymatic Hydrolysis of Phthalate Esters.

Determination of Phthalates in Polymer Materials Comparison of GC/MS and GC/ECD methods

Rapid and Simple Determination of Phthalates in Plastic Toys by a Thermal Desorption-GC/MS Method

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