HAYATSU Hikoya Shujitsu University, School of Pharmacy, Professor, 薬学部, 教授 (10012593)
MITANI Kurie Shujitsu University, School of Pharmacy, Research Associate, 薬学部, 助手 (70368702)
KIRA Shohei Okayama University, Graduate School of Medicine and Dentistry, Professor, 大学院・医歯学総合研究科, 教授 (50033212)
|Budget Amount *help
¥12,100,000 (Direct Cost : ¥12,100,000)
Fiscal Year 2004 : ¥1,700,000 (Direct Cost : ¥1,700,000)
Fiscal Year 2003 : ¥2,000,000 (Direct Cost : ¥2,000,000)
Fiscal Year 2002 : ¥8,400,000 (Direct Cost : ¥8,400,000)
Practical automated on-line analytical method for the determination of drugs and environmental pollutants was developed by in-tube solid-phase microextraction (SPME), in which these compounds were automatically extracted and concentrated using a capillary column as extraction device without organic solvent. Results of research for three years are as follows.
1.Endocrine disruptors such as phthalate esters were concentrated 18-125 times by in-tube SPME/HPLC using a Supel-Q PLOT capillary column. Calibration curves were linear in 1-500 ng/mL, and the detection limit was 0.1-4 ng/mL. DBP, OP, DEHP were detected from several food samples, and it was found that these compounds were migrated from container plastic. DBP was also detected in infusion solutions and some liquid medicines, and shown to be readily eluted from the adhesive into water and alcohol, and to easily pass through the plastic. These results indicated that the source of the DBP was the adhesive used to affix the paper labels
, and DBP contaminated the infusion solutions by passing through the plastic.
2.In-tube SPME/HPLC method of phytoestrogens daidzein and genistein, was developed. This method is highly sensitive and can detect these isoflavones at ng/mL level. This method was successfully applied to the analysis of soybean foods without interference peaks. The recoveries of daidzein and genistein spiked into food samples were above 97%, and these compounds were detected in soybeans and their processed foods, but not detected in other beans.
3.A simple, rapid and sensitive method for the determination of five estrogens, estrone, 17 β-estradiol, estriol, ethynyl estradiol, and diethylstilbestrol, was developed using a fully automated method consisting of in-tube solid-phase SPME coupled with LC/MS/MS. Using this method, good linearity of the calibration curve was obtained in the range from 5 to 200 pg/mL. Detection limits of the five estrogens ranged from 0.5 to 3.7 pg/mL, and the in-tube SPME method showed 30〜150-fold higher sensitivity than the direct injection method. This method was applied successfully to the analysis of environmental water samples without any other pretreatment and interference peaks.
4.In-tube SPME/LC/MS methods of diazine and triazine herbicides and sulfonamide antibactericides were developed and applied to the analysis of environmental water samples.
5.A molecule recognition capillary having a highly selectivity and concentration effect for estrogens was developed.
6.The in tube SPME technique could be easily combined to LC/MS, CE and CE/MS.
On-line in tube SPME/HPLC and LC/MS methods developed in this study can completely automate from pre-treatment of sample to data analysis, and it is simple, rapid, solvent elimination, high sensitive and lower cost. Therefore, it is expected as a practical method in food, environmental and clinical analysis. In addition, it is possible to improve the extraction efficiency and selectivity by the development of new capillaries coated or packed with new materials. Less