To establish an analytical method for the determination of content and migration of silver in silver-loaded silicone rubber products by inductively coupled plasma mass spectrometry.
The 3 mL nitric acid and 2 mL hydrofluoric acid were used as digestion acid for pretreatment of silver content, which were digested by microwave digestion method. The migration was simulated with 0.07 mol/L hydrochloric acid solution,4% acetic acid and artificial saliva. After shaking at 40 ℃ for 24 h, the immersion solution was filtered, and the quantitative analysis was performed by inductively coupled plasma mass spectrometry.
The silver content had good linearity in the mass concentration range of 0–100 μg/L, the correlation coefficient (r) was 1.0000, the limit of detection was 0.0009 mg/kg, the limit of quantitation was 0.0029 mg/kg, and the recovery rates were 95.5%–102.2%. The relative standard deviations (RSDs) were 0.92%–2.25%. In 0.07 mol/L hydrochloric acid solution, 4% acetic acid solution and artificial saliva mimics, silver had good linearity in the mass concentration range of 0–100 μg/L, and the correlation coefficients (r) were greater than 0.9995. The limits of detection were 0.0002, 0.0012 and 0.0024 mg/kg, respectively. The limits of quantitation were 0.0006, 0.0036 and 0.0077 mg/kg, the recoveries were 92.3%–101.8%, and the RSD was 1.03%–2.67%. The total silver content of 22 samples was not detected to 9.76 mg/kg, and the detection rate was 81.8%. The migration results of 4% acetic acid solution, 0.07 mol/L hydrochloric acid solution and artificial saliva were not detected to 0.0767 mg/kg, not detected to 0.1061 mg/kg and not detected to 0.0270 mg/kg, respectively, and the detection rates were 22.7%, 45.5% and 9.1%, respectively.
This method is convenient, sensitive, accreted and is suitable for quantitative analysis of total content and migration of silver in silicone rubber.
| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |