RESUMO
Objective: To establish a high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS)method for the determination of trivalent arsenic(AsIII),pentavalent arsenic(As), methyl arsenic(MA),dimethyl arsenic(DMA),arsenical choline(AsC)and arsenical betaine(AsB)in traditional Chi- nese medicine Cordyceps. Methods: The arsenic species in Cordyceps were extracted with hot 0.15 mol/L nitric acid so- lution,separated by HPLC on a Dionex IonPacTM AS7 column(4 mm×250 mm,5 μm)with aqueous 5 mmol/L and 100 mmol/L ammonium carbonate solutions in a gradient elution as mobile phase,and quantitatively determined by ICP-MS. Results: The six kinds of arsenic species showed a good linearity within the range of 5-200 μg/kg. The average recovery was 83.3-115.9%,and the relative standard deviation was less than 5%. The main form of arsenic species in C ordyceps was inorganic arsenic(AsIIIand As),and the total content of ASIII+Asvaried around 1 mg/kg in the three tested batches of samples. Conclusion: The established HPLC-ICP-MS method is convenient,accurate and reliable for the analysis of different arsenic species in Cordyceps. In addition,the present work on the determination of six arsenic species in Cordy- ceps could be used as reference for improvement of the limitation standard of arsenic in Cordyceps.
RESUMO
Objective To establish an analysis method for the detection of 6 arsenic compounds [AsC, AsB, As(Ⅲ), DMA, MMA and As(V)] in blood and urine by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry(HPLC-ICP-MS), and apply it to real cases. Methods Triton was used to damage cells, and then EDTA·2Na·2H2O was used to complex arsenic compounds in cells, and sonication and protein deposition by acetonitrile were performed for sample pretreatment. With the mobile phase consisted of ammonium carbonate and ultrapure water, gradient elution was per-formed for obtaining the arsenic compounds in samples, which were analysed by ICP-MS with Hamilton PRP-X100 column. Results The limits of detection in blood were 1.66-10 ng/mL, while the lower limits of quantitation in blood ranged from 5 to 30 ng/mL. The limits of detection in urine were 0.5-10 ng/mL, while the lower limits of quantitation in urine were 5-30 ng/mL. The relative standard deviation of inter-day and intra-day precisions was less than 10%. This method had been successfully applied to 3 cases. Conclusion This study has established an analysis method for detecting 6 common arsenic compounds in blood and urine, which can be used to detect the arsenic compounds in the blood and urine from ar-senic poisoning cases as well as the patients under arsenic treatment.