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Food Analysis / ICPE-9800 Series Analysis of Trace Elements in Fish Sample with ICP-AES (ICP-OES) on ICPE-9800 Application News AD-0163 Experimental The sample used in this analysis was Fish Protein Certified Reference Material for Trace Metals (DORM- 4), from National Research Council Canada. There were two sets of preparation. The sample, 0.5 g, was placed in a digestion vessel followed by addition of 5.0 mL of concentrated nitric acid, 2.0 mL of hydrogen peroxide and 1.0 mL of water. The mixture was digested using microwave-assisted digestion system based on AOAC 999.10 procedure. After the digestion process, deionized water was added to the digested sample to a final total volume of 20.0 mL. The calibration standards were prepared from 1000 ppm copper (Cu), iron (Fe) and zinc (Zn) standards, and 100 ppm ICP multi-element standard solution IX, which contains arsenic (As), cadmium (Cd), chromium (Cr), nickel (Ni), lead (Pb) and selenium (Se). The standard solutions were purchased from Merck Millipore, Germany. Type E-1 ultra pure water with resistivity of 18 ΩW was used. Three different calibration ranges were prepared to cover the range of the elements based on the certified values. The calibration standards were acid matched to the digested samples. Measurement was conducted using the Shimadzu ICPE- 9820 simultaneous ICP-AES spectrometer, equipped with the mini-torch. Table 1. Instrument and measurement conditions Instrument : ICPE-9820 Radio Frequency Power : 1.20 (kW) Plasma Gas Flow Rate : 10.0 (L/min) Auxiliary Gas Flow Rate : 0.60 (L/min) Nebulizer Gas Flow Rate : 0.70 (L/min) Nebulizer : Coaxial Nebulizer Spray Chamber : Cyclone Chamber Plasma Torch : Mini-torch Observation : Axial Introduction Fish is one of the most important food resource that is widely consumed in many parts of the world due to its high protein content, low saturated fats and omega-3 fatty acid. It is also rich in calcium and phosphorus. However, because of industrial discharges from human activities, fish may have trace levels of toxic elements such as arsenic, cadmium and lead which are absorbed from the environmental water and the foods they eat. The toxicity of these metals poses a concern to human health through the consumption of fish. Here, Shimadzu ICPE-9820, a simultaneous inductively coupled plasma atomic emission spectrometer (ICP-AES) was used to conduct a simultaneous analysis of elements in fish. The ICPE-9820, with its mini-torch plasma and spectrometer permitting all elements / all wavelengths simultaneous analysis, provides high sensitivity and throughput measurement while reducing running cost. The typical measurement conditions are shown in Table 1. The elements, wavelength and calibration ranges used are shown in Table 2. Element Wavelength Concentration Range As 193.759 0 to 0.2 ppm Cd 214.438 Cr 205.552 Ni 231.604 Pb 220.353 Se 203.985 Cu 224.700 0 to 2 ppm Zn 206.200 Fe 239.147 0 to 20 ppm Table 2. Elements, wavelength and calibration ranges
Application News AD-0163 SHIMADZU (Asia Pacific) Pte. Ltd 79 Science Park Drive, #02-01/08 Cintech IV, Singapore 118264 www.shimadzu.com.sg Tel: +65-6778 6280 Fax: +65-6778 2050 Copyright © 2017 SHIMADZU (Asia Pacific) Pte. Ltd. All rights reserved. No part of this document may be reproduced in any form or by any means without permission in writing from SHIMADZU (Asia Pacific) Pte. Ltd. Table 3. Quantitation results of Fish CRM DORM-4 on ICPE-9800 *Instrument Detection limit (IDL) is calculated as three times the standard deviation of 10 replicate measurements of a calibration blank Figure 1. Spectral Profiles of different elements on ICPE-9800 50 100 150 200 250 0.2 mg/L Standard 250 500 Samples 0.05 mg/L Standard Samples 0 500 1000 1500 205.50 205.55 205.60 Samples 0.2 mg/L Standard 0 2500 5000 7500 224.65 224.70 224.75 Samples 2 mg/L Standard 0 1000 2000 3000 239.10 239.15 239.20 Samples 20 mg/L Standard 0 1000 2000 Samples 0.2 mg/L Standard 200 300 400 Samples 0.05 mg/L Standard 100 150 200 250 Samples 0.2 mg/L Standard 0 5000 10000 Samples 2 mg/L Standard Conclusions The ICPE-9800 can provide simultaneous analysis of trace elements in fish CRM sample with high accuracy, which include low concentrations of Cd and Pb. Intensity Intensity Intensity Intensity Intensity Intensity Intensity Intensity Intensity Cd 214.438nm Cr 205.552nm Cu 224.700nm Fe 239.147nm Ni 231.604nm Pb 220.353nm Se 203.985nm Zn 206.200 As 193.759nm Element Fish CRM DORM-4 IDL (ppm)* Measured Value (mg/kg) (Duplicate) Measured Value (mg/kg) Certified Value (mg/kg) As 6.7 6.6 6.80 ± 0.64 0.008 Cd 0.298 0.303 0.306 ± 0.015 0.0002 Cr 1.85 1.76 1.87 ± 0.16 0.0007 Cu 15.1 15 15.9 ± 0.9 0.002 Fe 336 323 341 ± 27 0.03 Ni 1.24 1.29 1.36 ± 0.22 0.0004 Pb 0.43 0.45 0.416 ± 0.053 0.002 Se 3.7 3.8 3.56 ± 0.34 0.01 Zn 51.7 49.4 52.2 ± 3.2 0.0003 Results and Discussion The quantitative results for the trace elements were within the certification range of Fish Protein CRM DORM-4 as shown in Table 3. The spectral profiles of standards and samples are displayed in Figure 1. For Research Use Only. Not for use in diagnostic procedures.