Multiwalled carbon nanotubes as sorbent for on-line coupling of solid-phase extraction to high-performance liquid chromatography for simultaneous determination of 10 sulfonamides in eggs and pork.

The sulfonamides (SAs) have been widely used as effective chemotherapeutics and growth promoters in animals' feeding, but their residues could be a potential danger to human health due to their carcinogenic potency and possible antibiotic resistance. Development of a simple and sensitive method for the determination of SAs residues in food of animal origin, therefore, is of great significance. An on-line solid-phase extraction (SPE) method using multiwalled carbon nanotubes as sorbent coupled with high-performance liquid chromatography (HPLC) for simultaneous determination of 10 sulfonamides (SAs) in eggs and pork was developed. The adsorptive potential of carbon nanotubes for solid-phase extraction of sulfonamides was investigated for the first time in the present paper. To on-line interface solid-phase extraction with HPLC, a conventional sample loop on the six-port injector valve of the HPLC was replaced by a preconcentration column packed with carbon nanotubes. The analytes in water solution were preconcentrated onto the preconcentration column and subsequently eluted with mobile phase of methanol-water (22:78). The developed on-line solid-phase extraction method for HPLC permitted the current HPLC separation and the next preconcentration proceeded in parallel, and thus allows one determination finished within 35 min. The RSD of 10 SAs for nine replicate measurements of a standard mixture of 1 microgl(-1) were in the range of 2.5-7.8%. The method was applied to the determination of trace sulfadiazin (SDZ), sulfamerazine (SMR), sulfadimidine (SDMD), sulfathiazole (STZ), sulfamoxol (SMO), sulfamethizole (SMT), sulfamethoxypyridazine (SMP), sulfachlorpyridazine (SCP), sulfadoxin (SDX) and sulfisoxazole (SIA) in eggs and pork. The results indicated that the proposed method was simple, cost-effective and sensitive.

An ion-imprinted functionalized silica gel sorbent prepared by a surface imprinting technique combined with a sol-gel process for selective solid-phase extraction of cadmium(II).

A new ion-imprinted thiol-functionalized silica gel sorbent was synthesized by a surface imprinting technique in combination with a sol-gel process for selective on-line, solid-phase extraction of Cd(II). The Cd(II)-imprinted thiol-functionalized silica sorbent was characterized by FT-IR, the static adsorption-desorption experiment, and the dynamic adsorption-desorption method. The maximum static adsorption capacity of the ion-imprinted functionalized sorbent was 284 micromol g(-1). The largest selectivity coefficient for Cd(II) in the presence of Pb(II) was over 220. The static uptake capacity and selectivity coefficient of the ion-imprinted functionalized sorbent are higher than those of the nonimprinted sorbent. The breakthrough capacity and dynamic capacity of the imprinted functionalized silica gel sorbent for 4 mg L(-1) of Cd(II) at 5.2 mL min(-1) of sample flow rate were 11.7 and 64.3 micromol g(-1), respectively. No remarkable effect of sample flow rate on the dynamic capacity was observed as the sample flow rate increased from 1.7 to 6.8 mL min(-1). The imprinted functionalized silica gel sorbent offered a fast kinetics for the adsorption and desorption of Cd(II). The prepared ion-imprinted functionalized sorbent was shown to be promising for on-line, solid-phase extraction coupled with flame atomic absorption spectrometry for the determination of trace cadmium in environmental and biological samples. All competitive ions studied did not interfere with the determination of Cd(II). With a sample loading flow rate of 8.8 mL min(-1) for 45-s preconcentration, an enhancement factor of 56, and a detection limit (3sigma) of 0.07 microg L(-1) were achieved at a sampling frequency of 55 h(-1). The precision (RSD) for 11 replicate on-line sorbent extractions of 8 mug L(-1) Cd(II) was 0.9%. The sorbent also offered good linearity (r = 0.9997) for on-line, solid-phase extraction of trace Cd(II).