title: Chromatographic behavior of cadmium in an ion-pair reversed-phase micro HPLC system and its application to the determination of bio-available cadmium in soil samples.
abstract: A novel reversed phase ion-pair micro HPLC system with on-line fluorescence detection has been developed systematically and studied for the determination of cadmium in its bio-available fractions of soil samples. In this system, a micro ODS column of 1.0 mm i.d.x150 mm length and a mobile phase containing 6 mmol L(-1) 8-hydroxyquinoline 5-sulphonic acid (HQS), 3 mmol L(-1) cetyltrimethylammonium bromide (CTMABr), 10 mmol L(-1) acetic acid-acetate buffer (pH 5.1) as well as 50% acetonitrile at 50 microL min(-1) flow rate were employed to determine cadmium with a 2 microL flow cell through its fluorescence at 518 nm under 338 nm excitation. Furthermore, the composition of Cd-HQS chelate formed on the column was confirmed to be [Cd(HQS)(2)](2-) through a log-log plot method, and then combined with the ion-pair reagent by the electrostatic force under the chromatographic condition proposed. With such a method, the detection limit of cadmium was 8.48 ng mL(-1) (3sigma) with 1 microL sample injection, and the linear range for the determination of cadmium was 30-800 ng mL(-1) (R(2)=0.992). This method has been successfully applied to determination of cadmium in its bio-available fractions of BCR-483 and soil samples without interference from other coexistent metal ions. The RSD (n=6) was less than 7.3%. The results were in agreement with the indicative value for BCR-483 and those for the soil samples obtained by ICP-MS with a pretreatment of bis(1,1,3,3-tetramethylbutyl) phosphinic acid extraction.
authors.affiliation: Department of Chemistry & the MOE Key Laboratory of Analytical Sciences, Xiamen University, 361005, Xiamen, China.
authors.forename: Bin
authors.initials: B
authors.lastname: Li
authors.forename: Qiuquan
authors.initials: Q
authors.lastname: Wang
authors.forename: Hua
authors.initials: H
authors.lastname: Yan
authors.forename: Limin
authors.initials: L
authors.lastname: Yang
authors.forename: Benli
authors.initials: B
authors.lastname: Huang
mesh_terms: D001682:Biological Availability; D002104:Cadmium / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004784:Environmental Monitoring / Q000379:methods*; D007477:Ions / Q000737:chemistry; D012987:Soil / Q000032:analysis*
chemical_list: D007477:Ions; D012987:Soil; D002104:Cadmium