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User Benefits Application News Measured intensity ratio Measured intensity ratio Measured intensity ratio Standard value (μg/g) Standard value (μg/g) Standard value (μg/g) Fig. 1 ALTRACE Calibration curves were prepared for cadmium (Cd), arsenic (As), and lead (Pb) using standard solutions for atomic absorption spectrophotometry adjusted to the four concentration levels shown below. Fig. 2 shows the calibration curves. Here, correction of the sample shape and matrix was done with scattered X-ray. In addition, correction for overlap of As by Pb was also carried out (coexisting element correction, dj method). Concentrations of calibration curve standard solutions: 0 (blank), 0.5, 1, 5 μg/g Calibration Curves Table 1 Lower Limits of Detection Control of hazardous heavy metals contained in foods and food additives is required in order to protect human health and safety. Therefore, various domestic laws and regulations (1)-(4) have been established in Japan, including “Standards and criteria for food and food additives, etc.” and “Japan’s Specifications and Standards for Food Additives”. From the viewpoint of sensitivity, the main technique used in analyses of toxic heavy metals is atomic absorption spectrophotometry. However, as disadvantages of this method, powder and solid samples must be dissolved in an acid such as nitric acid or hydrochloric acid, and advanced technology and know-how are required in the actual analysis. In contrast, fluorescent X-ray spectroscopy offers excellent convenience because analysis is possible as-is, without dissolving the specimens. Shimadzu’s new product, the ALTRACE, energy dispersive X-ray fluorescence spectrometer (Fig. 1), makes it possible to analyze toxic heavy metals with high sensitivity thanks to the increased output of the X-ray tube and optimization of the optical design. As an additional advantage, continuous analysis of a maximum of 48 samples is possible, contributing to improved analysis throughput. This Application News article introduces the following: 1. Analysis of cadmium (Cd) in rice 2. Analysis of arsenic (As) and lead (Pb) in food additives Introduction In comparison with the conventional technology, sensitivity was improved by high voltage X-ray tube and optimization of the optical design. Analysis throughput is improved because continuous analysis of a maximum of 48 samples is possible. Screening for hazardous elements in foods and food additives is possible with only simple sample preparation, such as loading the samples into the sample container. Screening Analysis for Hazardous Heavy Metals in Foods and Food Additives Kotomi Kuroda, Hirokazu Moriya Energy Dispersive X-ray Fluorescence Spectrometer ALTRACE Table 1 shows the lower limits of detection of each element calculated from the theoretical statistical variation of the calibration curves. Lower Limit of Detection Element Cd As Pb Analytical line CdKα AsKα PbLβ1 Lower limit of detection 0.08 0.08 0.10 Pb Cd As Degree of accuracy (σ) = 0.037 µg/g Degree of accuracy (σ) = 0.030 µg/g Degree of accuracy (σ) = 0.066 µg/g Fig. 2 Calibration Curves [μg/g]
Application News www.shimadzu.com/an/ Shimadzu Corporation © Shimadzu Corporation, 2025 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. See http://www.shimadzu.com/about/trademarks/index.html for details. Third party trademarks and trade names may be used in this publication to refer to either the entities or their products/services, whether or not they are used with trademark symbol “TM” or “”. 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. First Edition: Feb. 2025 01-00775-EN 1. Analysis of Cadmium in Rice Conclusion ALTRACE is a trademark of Shimadzu Corporation or its affiliated companies in Japan and/or other countries. The analytical sensitivity of the new Shimadzu ALTRACE was greatly improved by increasing the power of the X-ray tube and optimization of the optical design. As a result of this improved performance, ALTRACE is the optimum instrument for screening for hazardous elements in foods and food additives. In addition, because a large number of samples can be analyzed in a short time, ALTRACE also contributes to improved analytical throughput for the customer. <References> (1) Standards and criteria for food and food additives, etc. (1959, Ministry of Health and Welfare notification No. 370) (2) Public Health Bureau, Food Safety Standards and Evaluation Division notification No.0308-1, dated March 8, 2024 (3) Japan’s Specifications and Standards for Food Additives, 10 th Edition (4) CODEX GENERAL STANDARD FOR CONTAMINANTS AND TOXINS IN FOOD AND FEED (CODEX STAN 193-1995) Table 4 Analysis Conditions Sample White rice powder, certified reference material NMIJ CRM 7502-a Sample Preparation The sample was set in a sample cell lined with polypropylene film (thickness: 5 μm) and subjected to simple compression. Fig. 3 shows an image of the sample. Fig. 3 Image of Sample Fig. 4 CdKα Profile Cd Profile Fig. 4 shows the profile of CdKα. A peak can be observed clearly, even with a trace amount of cadmium (0.548 μg/g). Results of Repeatability Test Table 2 shows the results of a 10-time repeatability test. Table 2 Results of Repeatability Test Element Cd Standard value 0.548 Average value 0.532 Standard deviation 0.050 Coefficient of variation [%] 9.4 2. Analysis of Arsenic and Lead in Food Additive Sample • Adipic acid • L(+)-ascorbic acid (vitamin C) • Citric acid Sample Preparation The sample materials were set in a sample cell lined with polypropylene film (thickness: 5 μm) and subjected to simple compression. Due to the large grain shape of the citric acid, the sample material was crushed with a crushing machine. Results of Quantitative Analysis Table 3 shows the results of the quantitative analysis. Both arsenic and lead were below the lower limit of quantitation. Because the lower limit of quantitation is much lower than 1 μg/g, it can be understood that this analysis is effective for screening analysis of the organic samples listed in Japan’s Specifications and Standards for Food Additives. Table 3 Results of Quantitative Analysis * Element As Pb Adipic acid <0.21 <0.19 L(+)-ascorbic acid (vitamin C) <0.28 <0.17 Citric acid <0.28 <0.25 Analysis Conditions * The symbol “<” indicates that the result is below the lower limit of quantitation. The lower limit of quantitation is the theoretical 10 σ value. [μg/g] [μg/g] Instrument : ALTRACE Elements : Cd, As, Pb Analysis group : Quantitative analysis Analysis method : Calibration curve method Detector : SDD X-ray tube : Rh target Tube voltage : 50 [kV] (As, Pb) 65 [kV] (Cd) Tube current : Auto [μA] Primary filter : #1 (Cd), #5 (As, Pb) Atmosphere : Air Accumulation time : 300 [s] Dead time : Max. 40 % CdKα
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