高效液相色谱法测定化妆品中盐酸美满霉素等7种抗生素组分含量
色谱柱 | C18柱,250mm×4.6mm×5μm |
进样量 | 20μL |
流速 | 0.9mL/min |
流动相 | A:0.01mol/L草酸溶液(磷酸调节pH至2.0) B:甲醇 C:乙腈 A:B:C=69:11:20 |
柱温箱 | 30°C |
波长 | 268nm |
采集时间 | 22min |
各浓度峰面积 | ||||||
浓度mg/L 目标物 | 0.5 | 1 | 2 | 5 | 10 | 相关系数(R) |
盐酸美满霉素 | 19209 | 35658 | 86798 | 210697 | 425803 | 0.9998 |
甲硝唑 | 14665 | 28052 | 61921 | 139379 | 283241 | 0.9997 |
二水土霉素 | 26207 | 52125 | 107468 | 265766 | 540079 | 0.9999 |
盐酸四环素 | 19744 | 39705 | 82312 | 204106 | 413922 | 0.9999 |
盐酸金霉素 | 10137 | 20219 | 43603 | 113420 | 237213 | 0.9998 |
盐酸多西环素 | 9833 | 20726 | 47460 | 118973 | 249209 | 0.9998 |
氯霉素 | 13869 | 30459 | 67009 | 168390 | 347240 | 0.9999 |
浓度mg/L 目标物 | 1 | 2 | 3 | 4 | 5 | 6 | 7 | RSD |
盐酸美满霉素 | 0.912 | 0.964 | 0.956 | 0.946 | 0.990 | 0.972 | 0.931 | 2.7% |
甲硝唑 | 0.920 | 0.930 | 0.921 | 0.924 | 0.925 | 0.925 | 0.925 | 0.4% |
二水土霉素 | 0.990 | 0.976 | 0.977 | 0.983 | 0.985 | 0.979 | 0.982 | 0.5% |
盐酸四环素 | 0.973 | 0.958 | 0.946 | 0.968 | 0.966 | 0.962 | 0.963 | 0.9% |
盐酸金霉素 | 0.965 | 0.939 | 0.941 | 0.945 | 0.929 | 0.926 | 0.920 | 1.6% |
盐酸多西环素 | 1.007 | 0.967 | 0.942 | 1.040 | 1.017 | 1.015 | 0.982 | 3.4% |
氯霉素 | 0.915 | 0.954 | 0.964 | 0.936 | 0.935 | 0.916 | 0.914 | 2.1% |
保湿乳加标 | 测得浓度mg/L | 回收率 | |||||
样品 | 加标-1 | 加标-2 | 加标-3 | 加标-1 | 加标-2 | 加标-3 | |
盐酸美满霉素 | ND | 9.24 | 9.17 | 9.22 | 92.4% | 91.7% | 92.2% |
甲硝唑 | 4.48 | 12.69 | 12.85 | 12.52 | 94.4% | 96.0% | 92.7% |
二水土霉素 | ND | 10.55 | 10.50 | 10.29 | 105.5% | 105.0% | 102.9% |
盐酸四环素 | ND | 9.04 | 9.14 | 8.89 | 90.4% | 91.4% | 88.9% |
盐酸金霉素 | ND | 8.88 | 8.85 | 8.99 | 88.8% | 88.5% | 89.9% |
盐酸多西环素 | ND | 22.56 | 22.81 | 22.88 | 104.6% | 107.1% | 107.7% |
氯霉素 | ND | 9.81 | 9.61 | 9.73 | 98.1% | 96.1% | 97.3% |
防晒乳加标 | 测得浓度mg/L | 回收率 | |||||
样品 | 加标-1 | 加标-2 | 加标-3 | 加标-1 | 加标-2 | 加标-3 | |
盐酸美满霉素 | ND | 8.89 | 8.81 | 8.85 | 88.9% | 88.1% | 88.5% |
甲硝唑 | 3.25 | 12.04 | 12.63 | 12.34 | 94.5% | 100.4% | 97.5% |
二水土霉素 | ND | 10.09 | 10.46 | 10.21 | 100.9% | 104.6% | 102.1% |
盐酸四环素 | ND | 8.73 | 9.20 | 8.80 | 87.3% | 92.0% | 88.0% |
盐酸金霉素 | ND | 8.60 | 9.31 | 8.88 | 86.0% | 93.1% | 88.8% |
盐酸多西环素 | 12.10 | 22.17 | 22.57 | 22.70 | 100.7% | 104.7% | 106.0% |
氯霉素 | ND | 9.81 | 9.61 | 9.45 | 98.1% | 96.1% | 94.5% |
1 | 2 | 3 | 4 | 5 | 6 | 7 | SD | MDL (mg/L) | LOQ (mg/L) | LOQ (mg/kg) | |
盐酸美满霉素 | 0.513 | 0.515 | 0.511 | 0.517 | 0.514 | 0.513 | 0.510 | 0.002 | 0.007 | 0.024 | 0.2 |
甲硝唑 | 0.466 | 0.467 | 0.467 | 0.470 | 0.486 | 0.469 | 0.469 | 0.007 | 0.021 | 0.069 | 0.7 |
二水土霉素 | 0.518 | 0.538 | 0.517 | 0.517 | 0.522 | 0.522 | 0.511 | 0.008 | 0.025 | 0.085 | 0.8 |
盐酸四环素 | 0.505 | 0.531 | 0.513 | 0.509 | 0.529 | 0.507 | 0.504 | 0.011 | 0.034 | 0.113 | 1.1 |
盐酸金霉素 | 0.440 | 0.468 | 0.463 | 0.479 | 0.532 | 0.469 | 0.448 | 0.030 | 0.090 | 0.299 | 3.0 |
盐酸多西环素 | 0.531 | 0.543 | 0.510 | 0.533 | 0.546 | 0.495 | 0.494 | 0.022 | 0.066 | 0.219 | 2.2 |
氯霉素 | 0.490 | 0.480 | 0.493 | 0.502 | 0.452 | 0.510 | 0.460 | 0.021 | 0.064 | 0.213 | 2.1 |