酒类产品、中药材等样品中锡的方法验证报告
15次样品空白荧光强度值IF | 609.5 | 609.7 | 602.8 | 601.5 | 605.5 |
607.9 | 613.2 | 612.4 | 617.4 | 617 | |
619.7 | 616.9 | 615.5 | 616.9 | 610.7 | |
标准偏差SD | 5.6171 | ||||
锡检出限DL,ng/mL | 0.10 |
15次样品空白荧光强度值IF | 139.9 | 139.3 | 140.9 | 137.1 | 133.9 |
134.7 | 134 | 135.8 | 133.2 | 132 | |
133.4 | 134.4 | 132.8 | 132.5 | 134.7 | |
标准偏差SD | 2.8048 | ||||
锡检出限DL,ng/mL | 0.24 |
天数 | 1d | 2d | 3d | 4d | 5d | 6d | 7d | 8d |
微波消解1 | 31.3049 | 28.1431 | 27.8347 | 26.6665 | 26.0939 | 25.7491 | 27.6731 | 27.3842 |
微波消解2 | 24.8229 | 22.3308 | 22.1244 | 21.8136 | 20.9173 | 20.3658 | 21.5997 | 21.8592 |
湿法消解1 | 36.5771 | 33.5938 | 34.4094 | 34.7389 | 33.4004 | 32.5256 | 33.9972 | 32.1680 |
湿法消解2 | 39.9525 | 36.7155 | 37.2921 | 36.974 | 34.8517 | 33.5972 | 34.5635 | 33.5841 |
测定次数 | 1 | 2 | 3 | 4 | 5 | 6 | RSD% |
测定低限 | 0.1668 | 0.1447 | 0.1744 | 0.1653 | 0.1401 | 0.1722 | 9.1 |
常见限量 | 4.1897 | 4.2134 | 4.0354 | 4.0247 | 3.9674 | 3.9880 | 2.6 |
一合适点 | 7.7947 | 8.0247 | 7.9468 | 8.0117 | 7.9750 | 8.0056 | 1.1 |
锡含量,ng/mL | 1 | 2 | 3 | 4 | 5 | 6 | 平均值 | RSD% |
酒1 | 3.2594 | 3.2787 | 3.2975 | 3.2629 | 3.2703 | 3.2965 | 3.2776 | 0.5 |
酒2 | 3.4853 | 3.5244 | 3.5076 | 3.4903 | 3.5377 | 3.5506 | 3.5160 | 0.7 |
酒3 | 2.2792 | 2.3761 | 2.387 | 2.3914 | 2.4325 | 2.4023 | 2.3781 | 2.2 |
酒4 | 0.227 | 0.209 | 0.230 | 0.197 | 0.221 | 0.194 | 0.213 | 7.2 |
酒5 | N.D. | N.D. | N.D. | N.D. | N.D. | N.D. | - | - |
锡含量,mg/kg | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 平均值 | RSD% |
甜菜碱 | 0.165 | 0.160 | 0.156 | 0.154 | 0.159 | 0.174 | 0.170 | 0.162 | 4.5 |
丹参 | 0.144 | 0.156 | 0.152 | 0.158 | 0.152 | 0.154 | 0.150 | 0.152 | 2.9 |
天麻 | 0.0206 | 0.0226 | 0.0250 | 0.0245 | 0.0194 | 0.0234 | 0.0232 | 0.0227 | 9.0 |
锡含量 | 原样,ng/mL | 加标样,ng/mL | 加标量,μL | 回收率,% |
酒1 | 3.5160 | 7.1650 | 200 | 91.2 |
3.5160 | 7.1478 | 200 | 90.8 | |
酒2 | 2.3781 | 4.3293 | 100 | 97.6 |
2.3781 | 4.3321 | 100 | 97.7 |
样品 | 质量,g | 测试浓度ng/mL | 加标量μL | 计算值mg/kg | 测定量ug | 回收率,% |
天麻 | 0.5197 | 0.2723 | - | 0.0262 | 0.0136 | - |
0.5204 | 0.5324 | 15 | 0.0512 | 0.0266 | 86.7 | |
0.4952 | 0.5772 | 15 | 0.0583 | 0.0289 | 101.6 | |
0.5151 | 2.0497 | 100 | 0.199 | 0.1025 | 88.9 |
样品 | 编号 | 质量,g | 定容体积,mL | 测试值,ng/mL | 换算值,mg/kg | 标示值,mg/kg |
柑橘叶 | 1 | 0.4595 | 50 | 36.5771 | 3.98 | 3.8±0.5 |
2 | 0.4807 | 50 | 37.0799 | 3.86 | ||
3 | 0.5097 | 50 | 39.9525 | 3.92 | ||
4 | 0.4982 | 50 | 39.9395 | 4.01 |