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STEP Temperature (˚C) Time (min) Power (W) 1 50 2 1000 2 30 3 0 3 180 25 1000 4 150 1 0 5 180 4 1000 6 180 15 1000 Application News No.J122 Inductively Coupled Plasma Mass Spectrometry Analysis of Heavy Metals in Pet Food Using the ICPMS-2030 LAAN-A-CP-E035 Q Introduction In Japan, a law related to ensuring the safety of pet food (the Pet Food Safety Law) was enacted on June 1, 2009. Based on this law, standards are prescribed regarding the raising and safekeeping of domestic animals, show animals, farm animals, and test animals respectively to ensure the health and safety of the animals, and at the same time to prevent the animals from causing people problems or harm. The manufacture, sale, and import of pet food not in accordance with the regulations are prohibited, and manufacturers, vendors, and importers must comply with the component standards. A ministerial ordinance regarding component standards for pet food was also enacted on March 1, 2012 in Japan. This ordinance specifies three heavy metals; cadmium, lead, and arsenic. Here, we introduce a simultaneous analysis performed on toxic elements in pet food using the Shimadzu ICPMS-2030 ICP mass spectrometer. Q Sample Commercially available pet food Q Sample Preparation We used the microwave digestion method that could decompose samples faster than the typically used wet digestion method. Since this method uses a closed vessel, it also has the advantage that loss of volatile elements such as arsenic is minimal. In this study, the sample was decomposed using the Milestone General ETHOS-One. 0.15 g of the sample, 0.5 mL of hydrochloric acid, and 6.5 mL of nitric acid were added to a quartz vessel of the microwave digestion system for sample preparation. The mixture was then decomposed by the microwave digestion system. After sample decomposition, pure water was added to bring the measurement solution to a volume of 30 mL. At this point, Ga, In, and Bi (at a 10 μg/L concentration in measurement solution) were added as the internal standard elements. The sample decomposition conditions are shown in Table 1. Table 1 Sample Decomposition Conditions Using the Microwave Digestion System for Sample Preparation Q Instrument and Analytical Conditions The Shimadzu ICPMS-2030 ICP mass spectrometer was used for the measurements. Table 2 shows the measurement conditions. In addition to providing high sensitivity, the ICPMS-2030 is equipped with a collision system using helium gas, which reduces interference from argon and chlorine significantly. Instrument : ICPMS-2030 High-frequency output : 1.2 kW Plasma gas flowrate : 8.0 L/min Auxiliary gas flowrate : 1.10 L/min Carrier gas flowrate : 0.60 L/min Nebulizer : Nebulizer 10 Chamber : Cyclone chamber (electronically cooled) Plasma torch : Mini torch Collision gas : He Table 2 Analytical Conditions
Unit As Cd Pb Standard value μg/g 15 1 3 Detection limit μg/g 0.002 0.0008 0.0003 Pet food quantitative result μg/g 0.053 0.054 0.068 Spike recovery rate % 99 100 102 Spike recovery rate (%) = { (Analysis value for the spike recovery test sample − Analysis value) / Spike concentration} × 100 Application News No. © Shimadzu Corporation, 2016 For Research Use Only. Not for use in diagnostic procedures. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country. The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu. Company names, product/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its affiliates, whether or not they are used with trademark symbol “TM” or “®”. Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own. The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject to change without notice. www.shimadzu.com/an/ J122 First Edition: Aug. 2016 p Analysis The calibration curve method was used for analysis of the three elements; cadmium, lead, and arsenic. To verify the analysis results, a spike recovery test sample was created by adding a standard solution of measurement elements after the sample decomposition. Quantitative analysis was performed in the same way using this sample. p Analytical Results Fig. 1 shows the calibration curves for the elements. Table 3 shows the analysis results. The detection limit is 1/1000th or less of the standard value, so the sensitivity was evidently sufficient. Further, with the favorable spike recovery rates obtained, the validity of the quantitative values was confirmed. p Conclusion Using the ICPMS-2030, it is possible to perform an analysis for controlling the heavy metals; cadmium, lead, and arsenic in pet food. [Reference] Ministerial ordinance regarding component standards for pet food (on April 28, 2009) The Japan's Ministry of Agriculture, Forestry and Fisheries, and the Ministry of the Environment, Ordinance No.1) Table 3 Analytical Results for Pet Food 0 10 Concentration (μg/L) 0 10 Concentration (μg/L) 0 10 Concentration (μg/L) 0 25 50 75 Intensity Intensity Intensity As 75 (2G) 0 10 20 30 40 50 Cd 114 (3N) 0 25 50 75 100 125 Pb 208 (3N) Fig. 1 Calibration Curves for As, Cd and Pb