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Abstract  

An on-line solid phase micro-column extraction and determination system for trace Cd and Pb in nuclear fuel grade uranium compounds was established. The preconcentration of trace elements Cd and Pb from uranium compounds was achieved by adsorbing Cd and Pb on CL-7301 resin in hydroiodic acid media, while the uranyl ion passed through. The method coupled with flame atomic absorption spectrometry (FAAS) was applied to analysis trace Cd and Pb in real samples. The preconcentration factors obtained by this method were 320 and 180 each for Cd and Pb, respectively. Under the optimized conditions, the detection limits corresponding to three times the standard deviation of the blank were found to be 0.13 ng·mL−1 and 0.37 ng·mL−1 for Cd and Pb, respectively. The relative standard deviation (RSD) and the recoveries of standard addition (spiked with 1–5 ng of Cd and Pb) were of <5% (n = 10) and 96.2%–102.3%, respectively. Precision was also evaluated and found to be ≤4.3% (N = 11). The proposed method was successfully used for the determination of trace Cd and Pb in commercially available uranium compounds (e.g., uranyl acetate and triuranium octoxide).

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Acta Chromatographica
Authors: Long Wang, Yuan-Yuan Jiang, Li Zhang, Tao Wang, Rui-Wu Yang, Chun-Bang Ding, Xiao-Li Wang, and Yong-Hong Zhou

A high-performance liquid chromatography (HPLC) method has been developed for the simultaneous identification and quantification of active compounds (cryptotanshinone, dihydrotanshinone I, tanshinone IIA, tanshinone I, salvianolic acid A, salvianolic acid B, protocatechuic aldehyde, and rosmarinic acid) contained in traditional Chinese folk medicine Salvia przewalskii Maxim. The herb samples (including wild, cultivated, and yin pian) from fourteen main regions were investigated. Chromatographic separation was performed on an Agilent Eclipse XDB-C18 reserved-phase column (250 mm × 4.6 mm i.d., 5 μm) using gradient elution with water-formic acid (99.9: 0.1, v/v) and acetonitrile at a flow rate of 0.8 mL min−1, an operating temperature of 30 °C, and a wavelength of 275 nm. Similarity analysis (SA), principal component analysis (PCA), and hierarchical cluster analysis (HCA) were used to analyze the data based on fingerprints. For fingerprint analysis, 27 peaks were selected as the common peaks to evaluate the similarities among different samples. The results of SA showed that the method permits to obtain desired linearity, precision, accuracy, and recovery. All samples were divided into three categories by PCA and HCA, and the concentration of the eight bioactive compounds varied significantly from different regions. It was demonstrated that chromatographic fingerprinting by HPLC combined with the simultaneous determination of eight bioactive compounds was a helpful method for the quality control of S. przewalskii.

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