表5.1 茶叶及茶叶浸泡液测定时ICP-MS仪器优化后的条件
仪器参数 | 数值 |
RF功率 | 1500W |
采样深度 | 8.0mm |
冷却气流量 | 15L/min |
辅助气流量 | 1.0 L/min |
载气流量 | 0.8 L/min |
补偿气流量 | 0.2L/min |
蠕动泵转速 | 0.1rps |
样品提取时间 | 45s |
稳定时间 | 60s |
积分时间 | 0.3s |
重复次数 | 3次 |
信号响应值cps | Y(89)≥8万 Tl(205)≥3万 |
Y、Tl信号响应值cps的RSD | <5% |
氧化物 | <1.2% |
采集模式 | 全谱模式 |
调谐模式 | no gas调谐模式 |
样品编号 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
茶叶稀土总量( ug/kg) | 2759 | 2967 | 3042 | 3039 | 5399 | 4069 | 3776 | 3409 | 2920 | 2530 |
溶出茶叶稀土总量(ug/kg) | 292 | 171 | 318 | 260 | 755 | 582 | 480 | 162 | 1018 | 370 |
稀土溶出率(%) | 10.6 | 5.8 | 10.5 | 8.6 | 14.0 | 14.3 | 12.7 | 4.8 | 34.9 | 14.6 |
表5.4 ***茶大红袍茶叶中16种稀土元素含量及浸泡液含量总量分布表
样品号 | 分析项目 | 45 Sc | 89 | 139 | 140 Ce | 141 Pr | 146 Nd | 147 Sm | 151 Eu | 157 Gd | 159 Tb | 162 Dy | 165 Ho | 166 Er | 169 Tm | 172 Yb | 175 Lu |
1 | 茶叶稀土 | 171 | 324 | 383 | 619 | 68.8 | 241 | 45.4 | 11.1 | 56.0 | 0 | 45.2 | 0 | 28.4 | 0 | 30.2 | 0 |
溶出稀土 | 5.9 | 21.7 | 36.7 | 108 | 6.0 | 24 | 4.1 | 4.4 | 16.4 | 0 | 4.3 | 0 | 2.7 | 0 | 2.7 | 0 | |
溶出率(%) | 3.5 | 6.7 | 10.0 | 17.4 | 8.7 | 10.0 | 9.0 | 39.6 | 29.3 | / | 9.5 | / | 9.5 | / | 8.9 | / | |
2 | 茶叶稀土 | 212 | 325 | 433 | 758 | 88.5 | 324 | 59.8 | 14.3 | 67.5 | 0 | 48.7 | 0 | 26 | 0 | 22.9 | 0 |
溶出稀土 | 18.6 | 44.6 | 17.7 | 44.5 | 3.4 | 15 | 2.8 | 0.9 | 3.7 | 0 | 2.8 | 0 | 1.9 | 0 | 1.5 | 0 | |
溶出率(%) | 8.8 | 13.7 | 4.1 | 5.9 | 3.8 | 4.6 | 4.7 | 6.3 | 5.5 | / | 5.8 | / | 7.3 | / | 6.6 | / | |
3 | 茶叶稀土 | 135 | 361 | 388 | 898 | 79.4 | 309 | 62 | 0 | 68.2 | 0 | 58.1 | 0 | 38.1 | 0 | 45.6 | 0 |
溶出稀土 | 4.7 | 30 | 31.9 | 129 | 6.5 | 27.8 | 5.6 | 0 | 7.8 | 0 | 5.5 | 0 | 3.8 | 0 | 4.1 | 0 | |
溶出率(%) | 3.5 | 8.3 | 8.2 | 14.4 | 8.2 | 9.0 | 9.0 | / | 11.4 | / | 9.5 | / | 10.0 | / | 9.0 | / | |
4 | 茶叶稀土 | 92.7 | 305 | 532 | 962 | 81.8 | 289 | 49 | 15.7 | 55.7 | 0 | 40 | 0 | 25.4 | 0 | 25.8 | 0 |
溶出稀土 | 13.9 | 15.4 | 36.8 | 86.4 | 5.6 | 21.4 | 4.0 | 4.7 | 16.2 | 0 | 2.9 | 0 | 1.7 | 0 | 1.5 | 0 | |
溶出率(%) | 15.0 | 5.0 | 6.9 | 9.0 | 6.8 | 7.4 | 8.2 | 29.9 | 29.1 | / | 7.3 | / | 6.7 | / | 5.8 | / | |
5 | 茶叶稀土 | 132 | 745 | 1008 | 1024 | 192 | 743 | 131 | 19.1 | 144 | 0 | 116 | 0 | 69.9 | 0 | 74.8 | 0 |
溶出稀土 | 1.4 | 40 | 60.3 | 248 | 10.1 | 168 | 7.6 | 3 | 47.3 | 0 | 11.8 | 0 | 15.7 | 0 | 5.3 | 0 | |
溶出率(%) | 1.1 | 5.4 | 6.0 | 24.2 | 5.3 | 22.6 | 5.8 | 15.7 | 32.8 | / | 10.2 | / | 22.5 | / | 7.1 | / | |
6 | 茶叶稀土 | 99.3 | 465 | 1161 | 582 | 126 | 470 | 92.3 | 91.1 | 92.8 | 0 | 78.7 | 0 | 46.7 | 0 | 57.2 | 0 |
溶出稀土 | 3.4 | 50.2 | 109 | 130 | 21.6 | 87.2 | 17.2 | 5.0 | 29.2 | 0 | 12.5 | 0 | 6.5 | 0 | 7.0 | 0 | |
溶出率(%) | 3.4 | 10.8 | 9.4 | 22.3 | 17.1 | 18.6 | 18.6 | 5.5 | 31.5 | / | 15.9 | / | 13.9 | / | 12.2 | / | |
7 | 茶叶稀土 | 119 | 421 | 831 | 747 | 141 | 522 | 85.2 | 0 | 93.4 | 0 | 66.8 | 0 | 32.9 | 0 | 33.7 | 0 |
溶出稀土 | 4 | 35.0 | 75.0 | 172 | 12.3 | 48.6 | 8.5 | 0 | 24.6 | 0 | 7.0 | 0 | 4.0 | 0 | 3.9 | 0 | |
溶出率(%) | 3.4 | 8.3 | 9.0 | 23 | 8.7 | 9.3 | 10.0 | / | 26.3 | / | 10.5 | / | 12.2 | / | 11.6 | / | |
8 | 茶叶稀土 | 93.4 | 301 | 1490 | 414 | 69.7 | 81.0 | 43.6 | 0 | 46.7 | 0 | 37.2 | 0 | 22.2 | 0 | 22.6 | 0 |
溶出稀土 | 11.2 | 11.0 | 13.0 | 72.5 | 2.8 | 13.4 | 2.5 | 0 | 9.7 | 0 | 2.5 | 0 | 1.8 | 0 | 1.5 | 0 | |
溶出率(%) | 12.0 | 3.7 | 0.9 | 17.5 | 4.0 | 16.5 | 5.7 | / | 20.8 | / | 6.7 | / | 8.1 | / | 6.6 | / | |
9 | 茶叶稀土 | 90.1 | 387 | 752 | 501 | 95.2 | 351 | 55.3 | 0 | 62.7 | 0 | 48.5 | 0 | 26.1 | 0 | 25.3 | 0 |
溶出稀土 | 20.5 | 47.7 | 57.5 | 52.2 | 8.5 | 70.4 | 6.8 | 0 | 6.8 | 0 | 6.4 | 0 | 8.2 | 0 | 3.3 | 0 | |
溶出率(%) | 22.8 | 12.3 | 7.7 | 10.4 | 8.9 | 20.1 | 12.3 | / | 10.8 | / | 13.2 | / | 31.4 | / | 13.0 | / | |
10 | 茶叶稀土 | 44.9 | 151 | 76.5 | 1184 | 52.6 | 192 | 22.1 | 0 | 29.5 | 0 | 15.1 | 0 | 0 | 0 | 0 | 0 |
溶出稀土 | 4.0 | 55.4 | 31.5 | 169 | 5.4 | 20.8 | 3.4 | 0 | 6.1 | 0 | 2.9 | 0 | 0 | 0 | 0 | 0 | |
溶出率(%) | 8.9 | 36.6 | 41.2 | 14.3 | 10.3 | 10.8 | 15.4 | / | 20.7 | / | 19.2 | / | / | / | / | / | |
平均溶出率(% | 8.2 | 11.1 | 10.3 | 15.8 | 8.2 | 12.9 | 9.9 | 9.7 | 21.8 | 0 | 10.7 | 0 | 12.2 | 0 | 8.1 | 0 |