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Operator care and eco-concerned development of a fast, facile and economical assay for basic nitrogenous drugs based on simplified ion-pair mini-scale extraction using safer solvent combined with drop-based spectrophotometry.

Talanta (2012-09-04)
Samarwadee Plianwong, Areerut Sripattanaporn, Kwanrutai Waewsa-nga, Parin Buacheen, Praneet Opanasopit, Tanasait Ngawhirunpat, Theerasak Rojanarata
ABSTRACT

A fast, facile, and economical assay for basic nitrogenous drugs has been developed based on the mini-scale extraction of the drug-dye ion pair complex combined with the use of safe-for-analyst and eco-friendlier organic extractant and drop-based micro-spectrophotometry. Instead of using large volume devices, the extraction was simply carried out in typical 1.5 mL microcentrifuge tubes along with the use of micropipettes for accurate transfer of liquids, vortex mixer for efficient partitioning of solutes and benchtop centrifuge for rapid phase separation. In the last step, back-extraction was performed by using the microvolume of acidic solution in order to concentrate the colored species into a confined aqueous microdrop and to keep the analyst away from unwanted contact and inhalation of organic solvents during the quantitation step which was achieved by using cuvetteless UV-vis micro-spectrophotometry without any prior dilutions. Using chlorpheniramine maleate as a representative analyte and n-butyl acetate as a less toxic and non-ozone depleting extractant, the miniaturized method was less laborious and much faster. It was accurate, precise and insensitive to the interferences from common excipients. Notably, it gave the assay results of drug in tablets and oral solution comparable to the large-scale pharmacopeial method while the consumption of organic solvents and the release of wastes were lowered by 200-400 folds.

MATERIALS
Product Number
Brand
Product Description

Supelco
Butyl acetate, Pharmaceutical Secondary Standard; Certified Reference Material
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Butyl acetate, ACS reagent, ≥99.5%
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Butyl acetate, ReagentPlus®, 99.5%
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Butyl acetate, suitable for HPLC, 99.7%
Supelco
Butyl acetate, analytical standard
Sigma-Aldrich
Butyl acetate, anhydrous, ≥99%
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Butyl acetate, ≥99%, FCC, FG
Sigma-Aldrich
Butyl acetate, natural, ≥98%, FG