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Shahana Huq

Publications and source records attributed to Shahana Huq.

2 recordsLinked to original sources

Role of zwitterionic structures in the solid-phase extraction based method development for clean up of tetracycline and oxytetracycline from honey.

Solid-phase extraction (SPE) based sample clean up of tetracycline (TC) and oxytetracycline (OTC) from honey samples was evaluated using a neutral polymeric sorbent (strata-X), a weak cation exchange polymeric sorbent (strata-X-CW) and a combination of neutral and strong cation exchange sorbents (strata-X plus Strata-Screen-C or strata-X-C). Both TC and OTC are recovered in low yields from the strong cation exchange sorbents strata-X-C and Strata-Screen-C under basic (pH >9) or acidic (pH >or=2) elution conditions. The cleanest extracts along with quantitative recoveries were obtained with strata-X-CW under either acidic or basic elution conditions, as demonstrated by analysis of eluates by both LC/UV and LC/MS-MS. On the other hand, the neutral sorbent (strata-X) was less efficient in eliminating the honey matrix constituents, since it could not retain the tetracyclines with the strong organic wash needed to remove other compounds. The differences in the elution behavior of the strong and weak cation exchange sorbents is rationalized on the basis of divergent deprotonation mechanisms of the tetracyclines, which exist in the zwitterionic structures under the SPE conditions.

Absorption↗

Novel solid-phase extraction protocol for 11-nor-9-carboxy-delta9-tetrahydrocannabinol from urine samples employing a polymeric mixed-mode cation-exchange resin, Strata-X-C, suitable for gas chromatography-mass spectrometry or liquid chromatography-mass spectrometry analysis.

A novel solid-phase extraction (SPE) method was developed for extraction and cleanup of 11-nor-9-carboxy-delta9-tetrahydrocannabinol (THC-COOH), the major metabolite of the active principle of marijuana, delta9-tetrahydrocannabinol, from urine samples. The protocol utilizes a polymeric mixed-mode cationic sorbent, Strata-X-C, which exhibits strong retention for the metabolite facilitating a more rigorous organic wash to eliminate matrix components/endogenous materials. Acetonitrile containing acetic acid was used as the elution solvent and is compatible with both LC-MS and GC-MS modes of analysis. The hydrophobic retention of Strata-X-C was demonstrated to be higher than a neutral polymeric sorbent, Strata-X, of the same backbone but devoid of the cation-exchange moiety (sulfonic acid), by LC studies employing homologous paraben probes. Simultaneously, the polar (non-ionic) interaction capability of Strata-X-C is also greater than that of Strata-X, as assessed through regioisomeric nitrophenol probes. These two features enable the metabolite to be retained strongly on Strata-X-C. Good linearity and precision was obtained for THC-COOH by GC-MS analysis of its trimethylsilyl derivative in the range 1-50 ng. A simplified room temperature instantaneous derivatization procedure was developed that is suitable for high-throughput screening of THC-COOH.

Cation Exchange Resins↗