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<p>Progress of drug risk assessment heavy metals and harmful elements in traditional Chinese medicine improving globally is slowed by limited understanding of heavy metals and harmful elements contents. This challenge becomes more complex when slight variations in measurement could affect the determination of heavy metals. The objectives of this study are to evealute the applicability of the existing standard methods suitable for determination heavy elements. A case study using two analytical methods, namely inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS), for the determination of lead and cadmium in PAEONIAE RADIX ALBA from two certified reference materials (ID: WPH240202024; ID: WPH240202025) with microwave digestion, wet digestion and dry ashing methods was conducted to evaluate their capacity to provide reliable and precise results. Instrument performance assessment was evaluated using limit of quantitation, limit of detection, precision, and calibration curve. Accuracy and precision of lead and cadmium contents were evaluated by the relative standard deviation. Based on the results of the two heavy elements, the analytical uncertainty has also been evaluated and the source of analytical uncertainty in all analytical and digestion methods was quantified identified. The results of the calibration curves for lead and cadmium of two analytical methods had a correlation coefficient greater than 0.999, which indicates that the linearity is good. The recovery rates for lead and cadmium using the two analytical methods ranged from 98.3% to 107.1%. The limit of quantitation for lead and cadmium of atomic absorption spectrometry was 0.09, 0.03&#xa0;mg/kg and of inductively coupled plasma mass spectrometry was 0.09, 0.03&#xa0;mg/kg. The limit of detection for lead and cadmium of atomic absorption spectrometry was 0.03, 0.01&#xa0;mg/kg and of inductively coupled plasma mass spectrometry was 0.03, 0.01&#xa0;mg/kg. Indicating that inductively coupled plasma mass spectrometry and atomic absorption spectrometry method exhibited excellent sensitivity. The results show compare relative standard deviation of the obtained results and certified values for lead and cadmium copper were 4%, 13% respectively. Such relative standard deviation to prove that accurate results could be obtained by using all the standard analytical methods with differently digestion methods for the reliable determination of the lead in <i>PAEONIAE RADIX ALBA</i>. Except for sample of dry ashing method using atomic absorption spectrometry detected cadmium that they are using inductively coupled plasma mass spectrometry and atomic absorption spectrometry technology the relative standard deviation is 3% (RSD% &lt; 5%) for microwave compare with wet digestion. For dry ashing digestion method proved unsatisfactory for the reliable determination of the cadmium in <i>PAEONIAE RADIX ALBA</i>. Also discussed is how to assess uncertainties related to sample mass, sample solution preparation, standard solution preparation process, and linear calibration curves. It has been observed that the calibration curve liner uncertainty is the most significant factor that contributes to the final uncertainty.</p>

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Measurement Uncertainty of Cadmium and Lead in PAEONIAE RADIX ALBA with AAS and ICP-MS: Comparison of Microwave Digestion, wet Digestion and Dry Ashing Approaches

  • 期刊论文

  • 发表日期：

    2026年4月24日

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  • Yingjuan Gao

摘要

Progress of drug risk assessment heavy metals and harmful elements in traditional Chinese medicine improving globally is slowed by limited understanding of heavy metals and harmful elements contents. This challenge becomes more complex when slight variations in measurement could affect the determination of heavy metals. The objectives of this study are to evealute the applicability of the existing standard methods suitable for determination heavy elements. A case study using two analytical methods, namely inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS), for the determination of lead and cadmium in PAEONIAE RADIX ALBA from two certified reference materials (ID: WPH240202024; ID: WPH240202025) with microwave digestion, wet digestion and dry ashing methods was conducted to evaluate their capacity to provide reliable and precise results. Instrument performance assessment was evaluated using limit of quantitation, limit of detection, precision, and calibration curve. Accuracy and precision of lead and cadmium contents were evaluated by the relative standard deviation. Based on the results of the two heavy elements, the analytical uncertainty has also been evaluated and the source of analytical uncertainty in all analytical and digestion methods was quantified identified. The results of the calibration curves for lead and cadmium of two analytical methods had a correlation coefficient greater than 0.999, which indicates that the linearity is good. The recovery rates for lead and cadmium using the two analytical methods ranged from 98.3% to 107.1%. The limit of quantitation for lead and cadmium of atomic absorption spectrometry was 0.09, 0.03 mg/kg and of inductively coupled plasma mass spectrometry was 0.09, 0.03 mg/kg. The limit of detection for lead and cadmium of atomic absorption spectrometry was 0.03, 0.01 mg/kg and of inductively coupled plasma mass spectrometry was 0.03, 0.01 mg/kg. Indicating that inductively coupled plasma mass spectrometry and atomic absorption spectrometry method exhibited excellent sensitivity. The results show compare relative standard deviation of the obtained results and certified values for lead and cadmium copper were 4%, 13% respectively. Such relative standard deviation to prove that accurate results could be obtained by using all the standard analytical methods with differently digestion methods for the reliable determination of the lead in PAEONIAE RADIX ALBA. Except for sample of dry ashing method using atomic absorption spectrometry detected cadmium that they are using inductively coupled plasma mass spectrometry and atomic absorption spectrometry technology the relative standard deviation is 3% (RSD% < 5%) for microwave compare with wet digestion. For dry ashing digestion method proved unsatisfactory for the reliable determination of the cadmium in PAEONIAE RADIX ALBA. Also discussed is how to assess uncertainties related to sample mass, sample solution preparation, standard solution preparation process, and linear calibration curves. It has been observed that the calibration curve liner uncertainty is the most significant factor that contributes to the final uncertainty.