JOURNAL OF COSMETIC SCIENCE 134 (Metuchen, NJ). A diluting solution of 1% HNO3 + 0.5 % HCl (v/v) was used for preparing calibration standards and analytical solutions. CALIBRATION STANDARDS FOR ICP-MS ANALYSES Calibration standards were prepared to contain the nominal concentration of each ele- ment to four signifi cant fi gures as shown in Table I. CALIBRATION STANDARDS FOR CVAFS MERCURY ANALYSES Mercury standards were prepared daily from dilution of the primary stock standard to 0.5, 1, 5, 2, and 40 ng/kg. A secondary check solution was made from dilution of the secondary stock standard to 5 ng/kg. Table XII. Elemental Results for 10 Foundations from 10 Manufacturers Manufacturer Brand Mean results (mg/kg)a As Cd Cr Co Pb Hg Ni A b TR NF 5.1 0.46 1.0 TR 0.73 B a TR NF 0.50 0.49 0.26 NF 0.99 C a TR NF 1.6 0.34 0.80 NF 0.96 E a 0.16 TR 1.4 1.2 1.2 NF 3.4 G a 0.31 NF 4.5 0.34 0.46 NF 1.6 K a TR NF 0.58 0.60 0.28 NF 1.3 N b TR NF 3.1 0.43 0.69 NF 1.1 P a 0.20 NF 3.5 2.5 0.70 NF 5.8 U a 0.19 NF 0.46 0.16 0.16 NF 0.56 V a 0.40 TR 2.4 1.1 0.82 TR 1.8 NF: Not found, or less than detection limit TR: Trace, or greater than detection limit, but less than quanti- tation level. a Mean results of duplicate determinations. Table XIII. Elemental Results for 5 Body Powders from 4 Manufacturers Manufacturer Brand Mean results (mg/kg)a As Cd Cr Co Pb Hg Ni E c 0.29 NF 3.9 1.4 1.5 NF 4.6 U c NF NF TR NF NF NF TR U d TR NF 1.9 1.1 0.11 NF 1.6 EE a 0.80 NF 0.29 0.073 0.56 NF 0.22 FF a 0.35 NF 1.7 1.6 0.21 NF 3.8 NF: Not found, or less than detection limit TR: Trace, or greater than detection limit, but less than quanti- tation level. a Mean results of duplicate determinations.
SURVEY OF COSMETICS FOR SEVEN INORGANIC ELEMENTS 135 SAMPLE DIGESTION PROCEDURE Prior to conducting the sample analyses, FDA asked Frontier to demonstrate reproduc- ible and accurate results for the seven analytes in seven reference lipsticks and four certi- fi ed reference materials with various matrices intended to mimic different cosmetic types (Conostan oil, marine sediment, tomato leaves, and fertilizer). This was done to demon- strate performance criteria for the limit of detection (LOD), limit of quantitation (LOQ), quality control (QC), and precision. The laboratory had previously performed analyses for FDA’s expanded study of lead in lipstick using the method developed and validated for that purpose (6,7). Frontier attempted to modify that digestion procedure to conduct the new analyses. However, they encountered diffi culties when the reported digestion proce- dure was applied to the new analytes and matrices. This prompted the development of a new sample preparation technique, described below. Sample digestions were performed in closed vessels with oven heating followed by re- peated evaporation (except for mercury analyses) of the acid mixture. The procedure used was as follows: • Weigh and transfer 0.5 ± 0.1 g analytical portion to a digestion vessel. • Add 25 ml of a 3:1 HNO3:HF mixture and 3 ml of HCl to the vessel. Table XIV. Elemental Results for 5 Compact Powders from 5 Manufacturers Manufacturer Brand Mean results (mg/kg)a As Cd Cr Co Pb Hg Ni A a 0.59 NF 16 4.4 6.8 0.0040 12 B a 0.28 NF 1.4 1.8 2.0 NF 3.9 C a 0.65 0.072 4.8 14 1.6 NF 28 E a 0.66 NF 11 0.82 7.8 TR 6.0 U a 0.34 NF 4.7 3.0 0.36 NF 8.7 NF: Not found, or less than detection limit TR: Trace, or greater than detection limit, but less than quanti- tation level. a Mean results of duplicate determinations. Table XV. Elemental Results for 5 Shaving Creams from 4 Manufacturers Manufacturer Brand Mean results (mg/kg) As Cd Cr Co Pb Hg Ni B c Product 1 NF NF 0.50 NF TR NF NF B c Product 2 TR NF 0.21 NF NF NF TR U a NF NF TR NF TR NF 0.13 CC b NF NF NF NF NF NF NF GG a TR NF TR NF NF NF NF NF: Not found, or less than detection limit TR: Trace, or greater than detection limit, but less than quanti- tation level. a Mean results of duplicate determinations.
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