Content overflows the browser. Try zooming out (Ctrl + −) to see the full page. PDF Download
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.J120 Inductively Coupled Plasma Mass Spectrometry Analysis of Minerals and Harmful Elements in Formula Milk Powder Using ICPMS-2030 LAAN-A-CP-E033 Q Introduction Formula milk powder is formulated to contain a good balance of minerals necessary for infant growth. Japan's Health Promotion Law includes stipulations on the essential mineral content, including calcium (Ca), iron (Fe), and copper (Cu), of food for special dietary use (e.g., formulated milk powder for infants) and requires the labeling of their content. 1) Harmful elements like lead (Pb) have a negative effect on infant development, and require strict safety controls from raw materials to the finished product. We describe using Shimadzu's ICPMS-2030 inductively coupled plasma mass spectrometer to perform a simultaneous analysis of elements present in formula milk powder (National Metrology Institute of Japan certified reference material [NMIJ CRM]). In addition to being highly sensitive, the ICPMS-2030 uses a helium gas collision system that greatly reduces the spectral interference caused by argon and chlorine. [References] 1) Permission standards for labeling and component composition of breast milk and formulated milk powder for infants (Permission for labeling of food for special dietary use, Food Labeling Division, Consumer Affairs Agency, No. 221 of March 31, 2016) Q Sample NMIJ CRM milk powder (for trace element analysis) (NMIJ CRM 7512-a: No. MI-040) Q Sample Preparation Compared to the normal wet digestion method, the microwave sample decomposition method has the advantages of completing decomposition in a shorter period of time and within a closed system, which results in little volatilization loss of As and other analytes. We used the ETHOS One (Milestone General K.K., Japan) to perform sample decomposition. After placing a sample 0.25 g, hydrochloric acid 0.5 mL, and nitric acid 6.5 mL in a quartz decomposition vessel, decomposition was performed using a microwave sample pretreatment system. After decomposition, pure water was added to make up 250 mL of solution for analysis (1000-fold dilution). At this point, Sc, Co, Ga, Y, In, and Ti internal standard elements were added (to an analytical solution concentration of 10 μg/L). Table 1 shows the decomposition conditions. Table 1 Decomposition Conditions for Microwave Digestion System Q Instrument and Analytical Conditions Shimadzu's ICPMS-2030 inductively coupled plasma mass spectrometer was used for analysis. Analytical conditions are shown in Table 2. In addition to being highly sensitive, the ICPMS-2030 uses a helium gas collision system that greatly reduces the spectral interference caused by argon and chlorine. 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 Sample introduction : Nebulizer 10 Chamber : Cyclone chamber (electronic cooling) Plasma torch : Mini-torch Collision gas : He Table 2 Analytical Conditions
Unit Measured Value (in Powder) NMIJ Certified Value Expanded Uncertainty Spike and Recovery (%) Ca g/kg 8.5 8.65 0.38 - Fe 0.102 0.104 0.007 - K 8.3 8.41 0.33 - Mg 0.82 0.819 0.024 - Na 1.81 1.87 0.09 - P 5.4 5.62 0.23 - Mn mg/kg 0.91 0.931 0.032 - Mo 0.230 0.223 0.012 - Sr 5.7 5.88 0.20 - Zn 41 41.3 1.4 - Cd <0.005 - - 100 Cr <0.06 - - 101 Pb <0.03 - - 100 As <0.03 - - 108 Spike and recovery (%) = { (Spike and recovery test sample analysis result - Measured value) / Spiked 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/ J120 First Edition: Sep. 2016 p Analysis Minerals and harmful elements present in formula milk powder were measured simultaneously using a calibration curve method. To confirm the validity of measured values, a spike and recovery test sample was prepared by adding a standard solution of analyte elements (Cd, Cr, Pb, As) after sample decomposition treatment. p Analytical Results Table 3 shows the analytical results. The results for mineral elements were within the range of certified levels, and good spike and recovery was obtained for trace amounts of harmful elements. p Conclusions We successfully used the ICPMS-2030 to simultaneously measure mineral constituents present in high concentrations in formula milk powder along with trace amounts of harmful elements. Table 3 Analytical Results for Certified Reference Material in Formula Milk Powder (NMIJ CRM 7512-a)