Solid-phase extraction and liquid chromatographic determination of monophthalates and phthalide extracted from solution administration sets.
A liquid chromatographic procedure is described for the determination of phthalide, monobutyl phthalate, and mono-2-ethylhexyl phthalate leached by water from solution administration sets. Recoveries varied from 88.8% for phthalide at 1 micrograms/50 mL to 113% for monobutyl phthalate at 6 micrograms/50 mL. Relative standard deviations at 1 micrograms/50 mL were 2.59% for phthalide, 3.54% for monobutyl phthalate, and 11.6% for mono-2-ethylhexyl phthalate. At 6 micrograms/50 mL, the relative standard deviation for mono-2-ethylhexyl phthalate decreased to 3.88%. Reproducibilities for 5 standard injections were 1.40% for phthalide, 1.84% for monobutyl phthalate, and 1.95% for mono-2-ethylhexyl phthalate. Correlation coefficients were 1.00 for the 3 compounds. Five sets from 2 manufacturers were examined. No phthalide or monobutyl phthalate was found. One manufacturer's sets contained 37.6-44.4 micrograms/L mono-2-ethylhexyl phthalate. The sample matrix had some interference if phthalide or monobutyl phthalate was present.
Snell
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U.S. Food and Drug Administration, Sterility Analysis Research Center, Minneapolis, MN 55401.
D001572:Benzofurans / Q000032:analysis*; D002853:Chromatography, Liquid; D004051:Diethylhexyl Phthalate / Q000031:analogs & derivatives* / Q000032:analysis; D007202:Indicators and Reagents; D007262:Infusions, Intravenous; D010795:Phthalic Acids / Q000032:analysis*; D012996:Solutions; D014867:Water / Q000032:analysis
D001572:Benzofurans; D007202:Indicators and Reagents; D010795:Phthalic Acids; D012996:Solutions; D014867:Water; C082022:phthalide; D004051:Diethylhexyl Phthalate; C016599:mono-(2-ethylhexyl)phthalate; C028577:monobutyl phthalate