Simultaneous determination of carbaryl and propanil in human serum and urine by on-line column-switching technique followed by automatic reversed-phase HPLC

Susumu Ichinoki, Natsuko Takido, Youichi Fujii, Toshihiro Morita, Ichiro Ieiri, Kenji Otsubo, Noriki Saitoh

Research output: Contribution to journalArticle

Abstract

Carbaryl and propanil in human serum and urine were determined by automatic on-line column enrichment technique followed by reversed-phase HPLC with photometric detection. Human serum was filtered through a membrane filter (0.45 micron pore size) and an aliquot of 0.1 ml of the filtrate was diluted with water up to 1 ml. The solution of 0.8 ml was directly injected to automatic HPLC without any preparation. Urine was incubated with beta-glucuronidase/arylsulfate for 16 hours at 37 degrees C. The resultant solution was then filtered through a membrane filter and the filtrate was analyzed by the similar manner as serum. Carbaryl and propanil in the sample solution were concentrated on a pre-conditioned ODS mini-column. After washing the mini-column with 5% methanol, they were separated by an ODS analytical column (Cosmosil 5 C18-MS, 250 x 4.6 mm i.d.) with acetonitrile/water (30:70, v/v) eluent and detected with a UV detector. Carbaryl and propanil in serum were detected at 220 and 210 nm, respectively. On the other hand, in order to separate from blank peaks, carbaryl and propanil in urine were detected at 290 and 260 nm, respectively. The presented HPLC method requires neither manual procedure of solid-phase nor liquid-liquid extraction. Calibration curves for carbaryl and propanil were linear over the range of 5 ng/ml-2 micrograms/ml in both serum and urine. Real serum (ng/ml level) and urine (microgram/ml level) samples were analyzed by the presented HPLC method. Effect of seventeen pesticides on the determination of carbaryl and propanil were investigated. All pesticides did not interfere with the determination except for thiuram.

Original languageEnglish
Pages (from-to)171-178
Number of pages8
JournalChūdoku kenkyū : Chūdoku Kenkyūkai jun kikanshi = The Japanese journal of toxicology
Volume16
Issue number2
Publication statusPublished - Jan 1 2003

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Propanil
Carbaryl
High Pressure Liquid Chromatography
Urine
Serum
Pesticides
Thiram
Liquid-Liquid Extraction
Membranes
Water
Glucuronidase
Calibration
Methanol

All Science Journal Classification (ASJC) codes

  • Medicine(all)

Cite this

Simultaneous determination of carbaryl and propanil in human serum and urine by on-line column-switching technique followed by automatic reversed-phase HPLC. / Ichinoki, Susumu; Takido, Natsuko; Fujii, Youichi; Morita, Toshihiro; Ieiri, Ichiro; Otsubo, Kenji; Saitoh, Noriki.

In: Chūdoku kenkyū : Chūdoku Kenkyūkai jun kikanshi = The Japanese journal of toxicology, Vol. 16, No. 2, 01.01.2003, p. 171-178.

Research output: Contribution to journalArticle

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AU - Otsubo, Kenji

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