Final report of the key comparison CCQM-K106: Pb, As and Hg measurements in cosmetic (cream)

Cosmetics are used in practically all walks of life as a means of improving skin and beautifying complexion. In recent years, more and more attention has been paid to the cosmetic safety. In response to the cosmetic safety issue, the accurate measurement of the heavy metals in cosmetics is, therefore, particularly important. NMIs from different countries should establish their chemical metrology traceability system in this area, which includes both measurement methods research and certain CRMs development. It should be noted that because the matrix of many cosmetics is complex and the contents of the heavy metals are relatively low, it still is a challenging task to measure the analytes with high accuracy and precision. CCQM-K106 followed up CCQM pilot study 'CCQM-P128: Pb, As measurements in cosmetic (cream)'coordinated by the National Institute of Metrology, China (NIM) in 2009. The cream was selected as the testing material, which is widely used as a daily skin care worldwide. This is the first CCQM key comparison regarding the measurement of toxic metal elements with the cosmetic matrix, which includes pure water, liquid paraffin, silicone oil, synthetic squalane, hyaluronic acid, glycerin, propylene glycol, allantoin, preservative and so on. The aim of the CCQM-K106 is to demonstrate the capability of participating NMIs and designated institutes in measuring the contents of poisonous elements, including lead, arsenic and mercury in a cosmetic sample (cream), and support CMC claims relating to inorganic elements in cosmetic materials and similar chemical industry products. The cream matrix sample was prepared under the guidance of professional technicians. The formula of the cream was carefully chosen to match with a real cosmetic. The homogeneity and stability level of Pb, As and Hg in the cream sample were fit for the objective of the comparison. Each participant received two numbered bottles containing about 5g samples in each bottle. The instruction relating to CCQM-K106 was sent to each participant by e-mail, which consisted of technical protocol, results report form and inorganic core capabilities tables. The results were reported as mass faction (mg/kg). Calculation of the uncertainty expressed as a combined standard uncertainty and an expanded uncertainty at 95% confidence. In order to allow a sufficient evaluation of the comparison, the report was required to include a detailed description of the applied method of measurement, information about sample digestion and preparation, information about the reference material used for calibration. The methods of measurement were free to be selected by the participants. For the sample treatment, most of the participants used microwave digestion method. For instrumental determination, a variety of techniques such as ICPMS, AAS, INAA were adopted by the participants. Most participants choose ID-ICP-MS method to measure Pb and Hg, which showed the better performance in terms of consistency and reliability of the measurement results. The reference mass fraction values and associated uncertainties were calculated by different statistic ways. As the result, the median and uncertainty of median were proposed as the key comparison reference value (KCRV) and its associated key comparison reference uncertainty after removal of suspected extreme values. In general, the performances of the majority of the CCQM-K106 participants are excellent, illustrating their measurement capability for Pb, As and Hg in a complex greasy matrix. The results can be used further by any participant to support its CMC claim at least for a borate buffer. That claim will concern the pH method employed by the participant during this comparison and will cover the used temperature(s) or the full temperature range between 15 degrees C and 37 degrees C for the participant which measured pH values at the three temperatures.