Rapid spectrophotometric determination of benzalkonium in pharmaceuticals by extraction/ FIA
Bivalent BPB anion reacts with 10-5 M quinine in neutral media to form a 1:2 charge transfer complex in 1, 2-dichloroethane, but not with 10-6 M benzalkonium. However, trace amounts of benzalkonium could be extracted into 1, 2-dichloroethane with BPB only when 10-410-5 M quinine was added in the ext...
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Published in | BUNSEKI KAGAKU Vol. 39; no. 2; pp. 73 - 77 |
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Main Authors | , , |
Format | Journal Article |
Language | Japanese English |
Published |
Tokyo
The Japan Society for Analytical Chemistry
1990
Japan Science and Technology Agency |
Subjects | |
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Abstract | Bivalent BPB anion reacts with 10-5 M quinine in neutral media to form a 1:2 charge transfer complex in 1, 2-dichloroethane, but not with 10-6 M benzalkonium. However, trace amounts of benzalkonium could be extracted into 1, 2-dichloroethane with BPB only when 10-410-5 M quinine was added in the extraction system giving a blue product. The molar absorptivity of the product was 50500 mol-1cm-1l at 610 nm. The blue product can be used for selective and rapid spectrophotometric determination of benzalkonium by the FIA method. The carrier solution (0.8 M phosphate buffer, pH 7.5) was pumped at a 0.75 ml/min flow rate and 1×10-4 M quinine standard solution and 5×10-5 M BPB were pumped at 0.25 ml/min each. Sample solutions (100 μl) were injected into the carrier stream by a six-way injection valve and mixed with the reagents in a 1 m reaction coil. The ion associate formed by quinine, BPB and benzalkonium was extracted into the organic phase in a 4 m extraction coil. The organic phase was separated by a phase separator with either a microporous polytetrafluoroethylene (PTFE) membrane (pore size 0.5 μm) or PTFE tubing (pore size 2 μm), and put through a 8-μl flow cell. Then the absorbance was measured at 610 nm and recorded as peak-shaped signals. Benzalkonium in the range of 5×10-6 M to 1.5×10-4 M could be determined and the relative standard deviation was 1.1% for 10 determinations of 1×10-4 M benzalkonium. The sample throughput was 24/h. The FIA method proposed here can be applied to the selective and rapid assay of benzalkonium in pharmaceuticals. |
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AbstractList | Bivalent BPB anion reacts with 10-5 M quinine in neutral media to form a 1:2 charge transfer complex in 1, 2-dichloroethane, but not with 10-6 M benzalkonium. However, trace amounts of benzalkonium could be extracted into 1, 2-dichloroethane with BPB only when 10-410-5 M quinine was added in the extraction system giving a blue product. The molar absorptivity of the product was 50500 mol-1cm-1l at 610 nm. The blue product can be used for selective and rapid spectrophotometric determination of benzalkonium by the FIA method. The carrier solution (0.8 M phosphate buffer, pH 7.5) was pumped at a 0.75 ml/min flow rate and 1×10-4 M quinine standard solution and 5×10-5 M BPB were pumped at 0.25 ml/min each. Sample solutions (100 μl) were injected into the carrier stream by a six-way injection valve and mixed with the reagents in a 1 m reaction coil. The ion associate formed by quinine, BPB and benzalkonium was extracted into the organic phase in a 4 m extraction coil. The organic phase was separated by a phase separator with either a microporous polytetrafluoroethylene (PTFE) membrane (pore size 0.5 μm) or PTFE tubing (pore size 2 μm), and put through a 8-μl flow cell. Then the absorbance was measured at 610 nm and recorded as peak-shaped signals. Benzalkonium in the range of 5×10-6 M to 1.5×10-4 M could be determined and the relative standard deviation was 1.1% for 10 determinations of 1×10-4 M benzalkonium. The sample throughput was 24/h. The FIA method proposed here can be applied to the selective and rapid assay of benzalkonium in pharmaceuticals. |
Author | SAKAI, Tadao MIYAJI, Toshihiko HIBI, Kiyokatu |
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References | 8) S. Motomizu, Y. Hazaki, M. Oshima, K. Toei : Anal. Sci., 3,265 (1987). 3) T. Sakai, N. Ohno : Chem. Lett., 1982,107. 11) 三瀬皓愛 : J. Flow. Inject. Anal., 5, 87 (1988). 1) H. M. N. H. Irving, J. J. Markham : Anal. Chim. Acta, 39, 7 (1967). 9) 酒井忠雄 : ぶんせき, 1987,260. 2) 金田吉男, 慶田雅洋 : 衛生化学, 22,370 (1976). 12) G. V. Scott : Anal. Chem., 40,768 (1968). 5) T. Sakai : Analyst (London), 108,608 (1983). 7) M. Tsubouchi : Bull. Chem. Soc. Jpn., 44, 1560 (1971). 4) T. Sakai : Anal. Chim. Acta, 147,331 (1983). 10) 本水昌二 : J. Flow Inject. Anal., 5, 71 (1988). 6) 酒井忠雄, 小島 聡, 佐伯栄二, 田中昌也 : 分析化学, 35,177(1986). |
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Snippet | Bivalent BPB anion reacts with 10-5 M quinine in neutral media to form a 1:2 charge transfer complex in 1, 2-dichloroethane, but not with 10-6 M benzalkonium.... |
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SubjectTerms | FIA coupled with solvent extraction formation of ternary ion associate by quinine, BPB and benzalkonium selective and rapid assay of benzalkonium in pharmaceuticals |
Title | Rapid spectrophotometric determination of benzalkonium in pharmaceuticals by extraction/ FIA |
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