1989 Fiscal Year Final Research Report Summary
Studies on Development of Polymeric Derivatizing Reagents for HPLC
| Project/Area Number |
63550566
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| Research Category |
Grant-in-Aid for General Scientific Research (C)
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| Allocation Type | Single-year Grants |
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| Research Field |
工業分析化学
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| Research Institution | Osaka University |
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Principal Investigator |
TANAKA Minoru Osaka Univ., Fac. Engr., Associate Professor, 工学部, 助教授 (60029238)
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| Project Period (FY) |
1988 – 1989
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| Keywords | Fatty acids / Derivatization / Polymeric reagents / HPLC |
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| Research Abstract |
1. Poly(4-nitrobenzyl p-styrenesulfonate), soluble in organic solvents, was synthesized and used as polymeric derivatizing reagent for HPLC with UV detection. By 4-nitrobenzylation with this reagent, C_8-C_<18> saturated fatty acids could be determined at concentrations down to 2.0 X 10^<-5> M. As a polymeric derivatizing reagent having a more sensitive labeling group than 4-nitrobenzyl, poly[2-(phthalimino)ethyl p- styrenesulfonate] was prepared. This reagent showed a lower determination limit of 1.0 X 10^<-6> M for C_<10>-Cl8 saturated fatty acids with UV detection.
2. Poly[2-(1-naphthyl)ethyl p-styrenesulfonate] was synthesized as the reagent with fluorescence detection, more sensitive than UV detection. With this reagent, C_6-C_<18> saturated fatty acids at 1.0 x 10^<-7> M could be determined. In order to obtain a more highly sensitive and reactive polymeric reagent, 2-(2,3-naphthalimino)ethyl group was selected. Its trifluoromethanesulfonate quantitatively converted the acids into the derivatives under quite mild conditions (at room temperatures for 10 min) and exhibited a determination limit of 1.0 x 10^<-8> M with fluorescence detection.
3. GC is more convenient than HPLC for the determination of lower saturated fatty acids. Therefore, copoly(pentafluorobenzyl p-styrenesulfonate-divinylbenzene), insoluble in solvents, was prepared. After pentafluorobenzylation with this reagent, C_4-C_8 saturated fatty acids could be determined at 1.0 X 10^<-7> M by GC with electron capture detection (ECD). This copolymeric reagent also readily pentafluorobenzylated inorganic anions of Br^-, I^-, SCN^- and S^<2-> in aqueous acetone. These anions at ppb levels could be determined with ECD.
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