This study aimed to develop a high-throughput HPLC-ICP-MS method for the simultaneous quantification of inorganic mercury (Hg²⁺) and methylmercury (MeHg⁺) in human breast milk. The method was validated using a certified reference material, achieving 99% accuracy.A 4-month analysis of breast milk samples from 10 participants examined the effects of collection method and timing on mercury speciation. The results revealed correlations between mercury species, fat content, and selenium, with MeHg⁺ concentrations being higher in hindmilk. The study highlights the importance of accurate mercury speciation and proper breast milk collection methodologies.<blockquote><h4>The original article</h4><h4><a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965">High-throughput mercury speciation analysis of breast milk using HPLC-ICP-MS</a></h4>Kenta Iwai, Miyuki Iwai-Shimada, Nozomi Tatsuta, Yayoi Kobayashi, Kaname Asato, Mitsuo Nishimoto, Kunihiko Nakai, Shoji F. NakayamaMicrochemical Journal, Volume 211, April 2025, 113142<a target="_blank" rel="noopener noreferrer" href="https://doi.org/10.1016/j.microc.2025.113142">https://doi.org/10.1016/j.microc.2025.113142</a><h6>licensed under <a target="_blank" rel="noopener noreferrer" href="https://creativecommons.org/licenses/by/4.0/">CC-BY 4.0</a></h6></blockquote>Selected sections from the article follow. Formats and hyperlinks were adapted from the original.<h3>1. Introduction</h3>Mercury is a global pollutant released into the oceans and atmosphere as a result of economic activities such as gold mining and natural phenomena such as volcanic eruptions <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0005" name="bb0005" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0005">[1]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0010" name="bb0010" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0010">[2]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0015" name="bb0015" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0015">[3]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0020" name="bb0020" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0020">[4]</a>. This element is present in the environment in various chemical forms, and the sources of exposure, health effects, and toxicokinetics differ significantly among chemical species; therefore, it is necessary to estimate the exposure level of each chemical species <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0025" name="bb0025" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0025">[5]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0030" name="bb0030" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0030">[6]</a>. Methylmercury (MeHg+), the chemical form of mercury of greatest concern in terms of human toxicity, is converted from inorganic mercury (Hg2+) by microorganisms, and individuals are exposed to it through the consumption of seafood. Nervous system disorders as well as cardiovascular and other effects have&nbsp;been reported&nbsp;following exposure to MeHg+ <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0035" name="bb0035" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0035">[7]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0040" name="bb0040" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0040">[8]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0045" name="bb0045" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0045">[9]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0050" name="bb0050" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0050">[10]</a>. The Minamata Convention on Mercury was established&nbsp;to regulate anthropogenic mercury emissions and advocate for the global monitoring of mercury exposure levels <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0055" name="bb0055" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0055">[11]</a>. Nevertheless, given that mercury remains a pervasive environmental pollutant, continuous global monitoring continues to be imperative.Exposure to mercury during the vulnerable period from the fetal stage to infancy is a health concern. Prenatal exposure to MeHg+ may adversely affect child development <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0060" name="bb0060" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0060">[12]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0065" name="bb0065" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0065">[13]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0070" name="bb0070" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0070">[14]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0075" name="bb0075" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0075">[15]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0080" name="bb0080" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0080">[16]</a>. Although measurements of total mercury in breast milk—the&nbsp;main&nbsp;source of exposure in infants—have been reported in many regions <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0085" name="bb0085" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0085">[17]</a>, MeHg+ <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0090" name="bb0090" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0090">[18]</a> and Hg2+ <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0095" name="bb0095" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0095">[19]</a> are released in breast milk; therefore, it is necessary to analyze these chemical species. Blood MeHg+ levels positively correlate with seafood consumption in Japan <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0100" name="bb0100" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0100">[20]</a>, <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0105" name="bb0105" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0105">[21]</a>, and inorganic mercury exposure is heavily influenced by dental amalgams <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0110" name="bb0110" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0110">[22]</a> and gold mining <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0115" name="bb0115" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0115">[23]</a>.&nbsp;In Japan,&nbsp;dental amalgams have rarely been used&nbsp;since the 1990s <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0120" name="bb0120" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0120">[24]</a>.&nbsp;In addition, Hg2+ exposure is also lower now because of the reduced use of mercury in thermometers and other devices.Thus fat, MeHg+ in breast milk has been analyzed mainly using gas chromatography equipped with electron capture detector (GC-ECD) <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0190" name="bb0190" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0190">[38]</a>; however, the&nbsp;pretreatment for such measurements is complicated, and the analytical volume required is large. It is especially important to establish a method that can adequately analyze even small amounts of colostrum because sample volumes are small. Consequently, the following prerequisites must be met for a comprehensive investigation of breast milk, including colostrum: 1) the minimum analytical volume of the sample must be feasible; 2) pretreatment must be straightforward; and 3) validation must be viable, with the methodology being proved highly reliable. In this study, we developed a high-throughput and sensitive analytical method for the separate determination of chemical species of mercury in breast milk that satisfies the above requirements.This study was designed to achieve three objectives. The first was to develop a straightforward approach for analyzing mercury speciation in breast milk. The second was to ascertain the impact of the sampling methodology and timing on the concentrations of Hg2+ and MeHg+ in breast milk. The third was to elucidate the relationships between the Hg2+ and MeHg+ contents and the contents of the other elements and fats.<h3>2. Methods</h3><h4>2.3. HPLC apparatus and conditions</h4>Separation was performed on a metal-free YMC-Triart C18 HPLC column (YMC CO., LTD., Kyoto, Japan), installed in an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=1260+Bio-inert+LC">Agilent 1260 Bio-inert LC</a> system consisting of a G5611A Bio-inert quaternary pump, G5611A Bio-inert high-performance autosampler, and a G1390B isocratic pump (Agilent Technologies Inc., Santa Clara, CA, USA). The outlet of the HPLC column was connected directly to an ICP-MS nebulizer (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#t0010" name="bt0010" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="t0010">Table 2</a>).<h4>2.4. ICP-MS device and conditions</h4>An <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=1&amp;search=8900+ICP-QQQ">Agilent 8900 ICP-QQQ </a>(Agilent Technologies Inc.) was used for speciation analysis and elemental concentration measurements. The introduction system consisted of a micro-mist nebulizer, a quartz double-pass spray chamber, and a quartz torch with a diameter of 2.5 mm. The total element concentration analysis was performed using the ICP-MS equipped with an SPS 4 Autosampler (Agilent Technologies, Inc.) [49].<h3>3. Results and discussion</h3><h4>3.2.3. Comparison of total mercury levels measured by HPLC-ICP-MS and ICP-MS</h4>To validate the developed method, we compared the sum of the Hg2+ and MeHg+ concentrations obtained using HPLC-ICP-MS with the total mercury concentration quantified via ICP-MS analysis. We analyzed foremilk and hindmilk samples from 10 participants in four sampling rounds (N = 80). The median concentrations (ng g−1) for the 80 samples were 0.109 (5th–95th percentile: 0.014–0.365) for Hg2+ and 0.220 (5th–95th percentile: 0.046–0.792) for MeHg+. The Hg2+ and MeHg+ concentrations in all the breast milk samples were above the MDL. The ICP-MS determination method for the total mercury and other elemental contents has been previously published <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#b0245" name="bb0245" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="b0245">[49]</a>. NIST SRM 1953 was used as the reference material to validate the determination of total mercury, as well as other elements using ICP-MS (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#s0120" name="bs0120" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="s0120">Supplemental Table 2</a>). No mercury chemical species other than Hg2+ and MeHg+ were present in breast milk, as determined by HPLC-ICP-MS; therefore, the sum of Hg2+ and MeHg+ was taken to be the total mercury in breast milk. To validate the analytical method, the distributions of total mercury as measured using HPLC-ICP-MS and ICP-MS were plotted. The results from the two methods were found to be strongly correlated (R2&nbsp;=&nbsp;0.895, Pearson’s correlation coefficient&nbsp;=&nbsp;0.946) (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#f0010" name="bf0010" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="f0010">Fig. 2</a> and <a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#s0120" name="bs0120" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="s0120">Supplemental Table 3</a>). The effects of adjusting the fat content were also investigated. The values showed better agreement in samples with low fat contents, whereas there was more variation in samples with high fat contents. For samples with high fat contents, the correlation improved upon fat content adjustment (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#s0120" name="bs0120" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="s0120">Supplemental Table 4</a>). A Bland–Altman plot was used to assess the agreement between the two methods (<a target="_blank" rel="noopener noreferrer" href="https://www.sciencedirect.com/science/article/pii/S0026265X25004965#f0015" name="bf0015" data-sd-ui-side-panel-opener="true" data-xocs-content-type="reference" data-xocs-content-id="f0015">Fig. 3</a>). The results of the two measurement methods were generally in agreement. However, discrepancies were observed at lower concentrations. These discrepancies are thought to be due to errors in the ICP-MS measurements, which increase as the measured concentration approaches the limit of quantification.<img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Microchemical_Journal_Volume_211_April_2025_113142_Fig_2_Regression_correlation_between_the_total_mercury_concentration_as_obtained_via_ICP_MS_analysis_02f63d9d9f.jpg" alt="Microchemical Journal, Volume 211, April 2025, 113142: Fig. 2. Regression correlation between the total mercury concentration as obtained via ICP-MS analysis and the sum of Hg2+ and MeHg+ as obtained via HPLC-ICP-MS analysis (N = 80). THg: total mercury." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Microchemical_Journal_Volume_211_April_2025_113142_Fig_2_Regression_correlation_between_the_total_mercury_concentration_as_obtained_via_ICP_MS_analysis_02f63d9d9f.jpg 168w," sizes="100vw" width="1400" height="1300"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/MICROC_3_c4a9ebef9e.jpg" alt="Microchemical Journal, Volume 211, April 2025, 113142: Fig. 3. A Bland–Altman plot and regression line (dotted line) and 95% limits of agreement (dashed lines) for total mercury in 80 samples as measured by ICP-MS and HPLC-ICP-MS." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_MICROC_3_c4a9ebef9e.jpg 156w," sizes="100vw" width="1400" height="1404"><h3>4. Conclusion</h3>We developed a high-throughput and sensitive method for analyzing mercury speciation in breast milk using HPLC-ICP-MS. The method was validated by analyzing NIST SRM 1953, comparing the values obtained with the total mercury concentrations obtained via ICP-MS analysis.&nbsp;Hg2+ and MeHg+ were detected in all the samples of foremilk and hindmilk provided monthly for 4&nbsp;months by the 10 participants. MeHg+ concentrations differed significantly between foremilk and hindmilk samples but not between samples obtained 2 and 5&nbsp;months postpartum. In contrast, Hg2+ concentrations in the foremilk and hindmilk did not differ and were correlated with selenium concentrations. Breast milk composition differs significantly between colostrum, transitional milk, and mature milk. Hence, a large cross-sectional study using our method will reveal the level of infant exposure to each chemical species of mercury.

High-throughput mercury speciation analysis of breast milk using HPLC-ICP-MS

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 22nd December 2025? Check out new documents from the field of spectroscopy/spectrometry and related techniques!<blockquote>👉 <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library">SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT SPECTROSCOPY/SPECTROMETRY RELATED TECHNIQUES</a></blockquote><blockquote>👉 Need info about different analytical techniques? Peek into <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library">LabRulezLCMS</a> or <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library">LabRulezGCMS</a> libraries.</blockquote>This week we bring you application notes by Agilent Technologies, Metrohm and Shimadzu!<h3>1. Agilent Technologies: Trace Elemental Analysis of Precursor Materials Using ICP-MS/MS</h3>Robust detection of Pt, Ag, Cd, and Ti in high-metal matrices using the <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=1&amp;search=8900+ICP-QQQ">Agilent 8900 ICP-QQQ</a> and reactive cell gases&nbsp;<ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_precursor_materials_8900_icp_ms_5994_8841en_agilent_81f1d8ffb5.pdf">Full PDF for download</a></li></ul>Precursor materials are fundamental to the fabrication of integrated circuits (ICs). In atomic layer deposition (ALD), they enable the controlled growth of ultrathin films on semiconductor substrates—an essential capability for scaling advanced device architectures. Because even trace metal impurities in precursors can degrade film performance and device yield, both suppliers and manufacturers routinely analyze these materials. Due to its sensitivity and multi-elemental capabilities, inductively coupled plasma mass spectrometry (ICP-MS) is the industry standard for assessing elemental impurities in semiconductor materials.1 However, the high concentration of the metallic (high-matrix) content of precursors and the prevalence of polyatomic and doubly charged ion (M++) spectral overlaps arising from the matrix on key analytes present challenges for accurate analysis by single-quadrupole ICP-MS. At one time, high-resolution (HR)-ICP-MS (m/Δm up to 10000) was the best choice for solving these kinds of analytical problems. But some interferences require a resolution that exceeds the capability of current HR-ICP-MS instruments. In these cases, the samples are sometimes diluted to reduce the concentration of matrix elements, but dilution cannot totally solve the interference and may negatively affect detection limits.&nbsp;Triple quadrupole ICP-MS (ICP-QQQ or ICP-MS/MS) combined with collision/reaction (CRC) gases overcomes these limitations by selectively removing or avoiding interferences without compromising sensitivity. Agilent ICP-QQQ systems use two quadrupoles (Q1 and Q2) as unit mass filters, enabling MS/MS operation and the controlled use of reactive cell gases. Q1 controls which ions enter the CRC and Q2 controls which ions reach the detector.2–4&nbsp;In this study, we evaluated the performance of the Agilent 8900 ICP-QQQ to determine key analytes in three simulated precursor materials. Each sample contained a highconcentration matrix of hafnium (Hf), zirconium (Zr), or molybdenum (Mo), which cause interferences on platinum (Pt), silver (Ag), and cadmium (Cd) and titanium (Ti), respectively. To demonstrate the 8900 ICP-QQQ system’s ability to remove spectral interferences without sacrificing sensitivity, we quantified the four analytes in the three matrices using optimized instrument operating conditions.<h4>Experimental</h4><h4>Instrumentation&nbsp;</h4>An <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=1&amp;search=8900+ICP-QQQ">Agilent 8900 Semiconductor configuration ICP-QQQ</a> (#200) fitted with the optional m-lens was used for all measurements. The 8900 #200 includes an inert (HF-resistant) sample introduction system comprising a 200 μL/min MicroFlow PFA nebulizer, a PFA spray chamber, endcap, and connector tube, and a demountable torch with a 2.5 mm internal diameter (id) sapphire injector. The cones comprised a Pt-tipped sampling cone and Pt-tipped, Ni-based skimmer cone for m-lens. The samples were self-aspirated using an Agilent SPS 4 autosampler. Hot plasma conditions (1% CeO+ /Ce+ ) were used during the analysis of the high-matrix samples.&nbsp;The 8900 ICP-QQQ was operated in MS/MS mode for all measurements. Ammonia (NH3 ) —plus a flow of helium (He) as a buffer gas—and oxygen (O2 ) were used as reactive cell gases to resolve the matrix-based interferences. Various CRC tuning modes and Q1–Q2 mass setting combinations were tested to obtain the best conditions for each analyte. The optimized operating conditions for the analysis are detailed in Table 1.<h4>Conclusion&nbsp;</h4>The Agilent 8900 Semiconductor configuration ICP-QQQ was evaluated for its ability to eliminate spectral interferences on four analytes—Pt, Ag, Cd, and Ti—in simulated semiconductor precursor materials using MS/MS and reactive cell gases. To accommodate challenging samples comprising Hf (500 ppm), Zr (500 ppm), and Mo (360 ppm) under hot plasma conditions (1% CeO+ /Ce+ ), the 8900 was equipped with the optional m-lens.&nbsp;Ammonia was applied in both on-mass and mass-shift modes to quantify Pt, Ag, and Cd at single-digit or sub-ppt levels. Oxygen on-mass mode effectively removed Mo-based doubly charged ion interferences on Ti, enabling accurate detection at single-digit ppt concentrations. Repeated analysis of the MoCl5 samples spiked at 50 ppt with %RSDs below 10% demonstrated the instrument’s robustness and consistent performance for ultratrace quantification in complex matrices.&nbsp;The 8900 ICP-QQQ delivered low background, high sensitivity, and reliable interference control, making it suitable for method development and trace-level screening of semiconductor materials.<h3>2. Metrohm: Fat content analysis in olive pomace with NIR spectroscopy</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_nir_137_download_bb86ed4a7f.pdf">Full PDF for download</a></li></ul>Olive pomace is the main residue of the olive oil extraction process. It is a thick sludge – the remaining pulpy material after most of the oil is removed from the olive paste. To extract the remaining oil it contains, the olive pomace is treated with solvents. After refining and mixing this with edible virgin olive oil for flavor, aroma, and color, olive pomace oil is obtained. Olive pomace oil is used in cooking for its milder flavor and stability at high temperatures [1], as well as being nutritionally relevant due to its high oleic acid content (C18:1) [2]. Olive pomace fat analysis is necessary to check the efficiency of the oil removal process. The official method to determine this requires a time-consuming drying step followed by solvent extraction. Near-infrared spectroscopy (NIRS) is a fast, chemical-free method for olive pomace testing without any sample preparation.<h4>EXPERIMENTAL EQUIPMENT</h4>140 samples of olive pomace were measured on a <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=56&amp;search=NIR+Analyzer">Metrohm NIR Analyzer</a>. All measurements were performed in reflection mode (1000–2250 nm) using the large cup accessory. The samples were measured in rotation to collect spectral data from several areas. Spectral averaging of signals from several spots helped to reduce sample inhomogeneity. Metrohm software was used for all data acquisition and prediction model development.<h4>RESULTS</h4>The obtained NIR spectra of olive pomace samples (Figure 1) were used to create a prediction model for quantification of fat content. The quality of the prediction model was evaluated using a correlation diagram (Figure 2) which displays a high correlation between the NIR prediction and the reference values measured with Soxhlet extraction. The respective figures of merit (FOM) display the expected precision of a prediction during routine analysis.<h4>CONCLUSION&nbsp;</h4>This Application Note shows the feasibility of using NIR spectroscopy for olive pomace fat analysis. By using NIRS, chemical-free analysis can be conducted within seconds—a quick, easy, cost-effective alternative to determine the efficiency of the olive pomace oil removal process.<h3>3. Shimadzu: Analysis of Pharmaceutical Raw Materials Compliant with ICH Q3D Guideline Using ICP-MS with Collision Mode</h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_01_00925_en_c760bf6c08.pdf">Full PDF for download</a></li></ul><h4>User Benefits</h4><ul><li>The 24 elements identified in the ICH Q3D guideline can be measured with high sensitivity.</li><li>Pharmaceutical raw materials that are dissolved in ethanol can be easily analyzed using the Shimadzu ICP-MS organic solvent system.</li></ul>The presence of impurities in pharmaceutical ingredients is a concern within the medical pharmaceutical industry. Therefore, the International Council on Harmonisation of Technical Requirementsfor Registration for Pharmaceuticalsfor Human Use requires the management of metallic impurities in pharmaceuticals through guidelines using ICP-MS (ICH Q3D) 1), 2) . This standard specifies the Permitted Daily Exposure (PDE) for 24 elements of toxicological concern in oral preparations, injectables, and inhalants.&nbsp;In the case of oral preparations, only the seven elements of Classes 1 and 2A are considered, except in instances where elements are intentionally added, such as when used as catalysts during synthesis. However, the sources of elemental impurities are diverse and include not only components such as active pharmaceutical ingredients and excipients but also manufacturing equipment and utensils.&nbsp;ICP-MS has the advantage of being able to analyze various trace elements simultaneously. It is often used for the analysis of elemental impuritiesin pharmaceuticals. The analyte for ICP-MS is usually a liquid sample, so solid samples require pretreatment.&nbsp;In this Application News, we measured three types of pharmaceutical raw materials and analyzed the impurities using the Shimadzu ICP-MS organic solvent system. Furthermore, the accuracy, precision, detection limits and specificity of 24 target elements are presented according to USP3), 4) and EP, assuming measurements below the Control Threshold of 30 % of the PDE.<h4>Instrument Configurations and Analysis Conditions&nbsp;</h4>Table 2 shows the instrument configuration for ICP-MS (<a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library?manufacturerItems=3&amp;search=ICPMS-2040">ICPMS-2040</a>). The organic solvent system was used to introduce the ethanol. By using the platinum sampling cone, damage from long-term exposure to organic solvents during analysis can be reduced. To reduce the labor required for sample preparation, the internal standards were added using the Online Internal Standard Kit. The analysis conditions are shown in Table 3.<h4>Accuracy and Precision Validation Results&nbsp;</h4>Measurements were carried out for n = 3 spiked samples with the target concentration of 50 % and 150 %, and n = 6 spiked samples with the target concentration and the blank (unspiked) sample. Spike recovery was calculated by averaging the quantitative values of all samples. Tables 6 to 8 show the measurement results.&nbsp;Accuracy: Spike recovery of the samples at each of the target concentrations of 50 %, 100 %, and 150 % was in the range of 94 % to 111 %, thereby satisfying the acceptance criterion. Precision (Repeatability): RSD of the spiked samples with the target concentration ranged from 0.27 % to 3.79 %, satisfying the acceptance criterion.&nbsp;Limit of quantitation: As accuracy for 50 % of the target concentration satisfied the acceptance criterion, the limit of quantitation could be confirmed.&nbsp;<h4>Specificity&nbsp;</h4>ICP-MS analysis often requires evaluation for potential interference by isotypes, polyatomic ions originating from Ar, oxides of coexistent elements and chloride ions. Here, the Cd was assessed. MoO, originating from the Class 3 element Mo, causes interference with Cd. A 1350 μg/L Mo solution (concentration equivalent to 1.5J) was analyzed, and the amount of interference with Cd was measured. Here, in addition to using collision gas, interelement correction was also performed. Table 5 shows the results.&nbsp;When the collision gas was used without interelement correction, interference by MoO was reduced but not eliminated. However, the quantitative value was below the lower limit of detection when the collision gas was used in combination with interelement correction. This result confirmed that the use of interelement correction, together with a collision gas, enables the appropriate correction of interference that could not be eliminated by the collision gas alone.<h4>Conclusion&nbsp;</h4>In this Application News, we measured three types of pharmaceutical raw materials and analyzed 24 elements indicated in the ICH Q3D guideline using the Shimadzu ICP-MS organic solvent system. In accordance with the pharmacopeias (USP, EP), the accuracy, precision, quantification limit, and specificity were confirmed. The results of the validation demonstrated that the performance meets the acceptance criteria with a sufficient margin. Based on the above, it was determined that the Shimadzu ICPMS-2040 is an effective analytical method for the 24-element analysis of pharmaceutical raw materials that can be dissolved in ethanol.

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