Laboratory Medicine ›› 2018, Vol. 33 ›› Issue (2): 132-138.DOI: 10.3969/j.issn.1673-8640.2018.02.009
• Orginal Article • Previous Articles Next Articles
YUE Xiaojing1, LI Wei2, LI Pingfa3
Received:
2017-03-12
Online:
2018-02-28
Published:
2018-03-02
CLC Number:
YUE Xiaojing, LI Wei, LI Pingfa. Determination of paraquat in plasma by HPLC-MS/MS[J]. Laboratory Medicine, 2018, 33(2): 132-138.
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URL: https://www.shjyyx.com/EN/10.3969/j.issn.1673-8640.2018.02.009
化合物 | 母离子>子离子 | 去簇电压(V) | 射入电压(V) | 碰撞电压(V) | 射出电压(V) |
---|---|---|---|---|---|
百草枯 | m/z 92.7→171.0 | 50 | 8 | 20 | 8 |
乙基百草枯 | m/z 107.0→185.1 | 22 | 7 | 14 | 16 |
化合物 | 母离子>子离子 | 去簇电压(V) | 射入电压(V) | 碰撞电压(V) | 射出电压(V) |
---|---|---|---|---|---|
百草枯 | m/z 92.7→171.0 | 50 | 8 | 20 | 8 |
乙基百草枯 | m/z 107.0→185.1 | 22 | 7 | 14 | 16 |
项目 | 准确度 | 精密度 | ||
---|---|---|---|---|
批内 | 批间 | 批内 | 批间 | |
定量下限 | 96.31 | 104.43 | 9.67 | 12.5 |
96.95 | 6.5 | |||
120.04 | 2.57 | |||
低浓度 | 88.07 | 93.93 | 10.4 | 11.1 |
102.33 | 5.43 | |||
91.4 | 12.4 | |||
中浓度 | 105.23 | 98.84 | 3.88 | 12.8 |
87.59 | 3.64 | |||
103.59 | 16.6 | |||
高浓度 | 102.17 | 91.36 | 13.5 | 13.8 |
82.26 | 8.83 | |||
89.64 | 8.57 |
项目 | 准确度 | 精密度 | ||
---|---|---|---|---|
批内 | 批间 | 批内 | 批间 | |
定量下限 | 96.31 | 104.43 | 9.67 | 12.5 |
96.95 | 6.5 | |||
120.04 | 2.57 | |||
低浓度 | 88.07 | 93.93 | 10.4 | 11.1 |
102.33 | 5.43 | |||
91.4 | 12.4 | |||
中浓度 | 105.23 | 98.84 | 3.88 | 12.8 |
87.59 | 3.64 | |||
103.59 | 16.6 | |||
高浓度 | 102.17 | 91.36 | 13.5 | 13.8 |
82.26 | 8.83 | |||
89.64 | 8.57 |
样本号 | 加入基质后 百草枯峰面积 | 溶液中百草枯峰面积 | 百草枯 基质因子 | 加入基质后 内标峰面积 | 溶液中内标 峰面积 | 内标 基质因子 | 内标归一化的基质因子 |
---|---|---|---|---|---|---|---|
低浓度 | |||||||
1 | 1.87×104 | 6.07×102 | 3.09×101 | 1.68×106 | 8.08×105 | 2.08×100 | 1.49×101 |
2 | 2.32×104 | 5.26×102 | 4.40×101 | 1.80×106 | 5.34×105 | 3.38×100 | 1.30×101 |
3 | 2.56×104 | 4.97×102 | 5.16×101 | 1.87×106 | 6.73×105 | 2.78×100 | 1.86×101 |
4 | 2.48×104 | 4.64×102 | 5.33×101 | 1.90×106 | 6.36×105 | 2.98×100 | 1.79×101 |
5 | 2.58×104 | 5.66×102 | 4.56×101 | 1.95×106 | 7.64×105 | 2.56×100 | 1.78×101 |
6 | 7.16×103 | 3.21×102 | 2.23×101 | 9.06×105 | 6.25×105 | 1.45×100 | 1.54×101 |
RSD | 1.33×101 | ||||||
高浓度 | |||||||
1 | 2.11×106 | 2.26×106 | 9.36×10-1 | 1.88×106 | 2.00×106 | 9.43×10-1 | 9.92×10-1 |
2 | 2.51×106 | 2.26×106 | 1.11×100 | 1.85×106 | 2.01×106 | 9.18×10-1 | 1.21×100 |
3 | 4.70×106 | 2.85×106 | 1.65×10-1 | 3.50×105 | 2.21×106 | 1.58×10-1 | 1.04×100 |
4 | 2.63×106 | 2.30×106 | 1.14×100 | 1.99×106 | 2.04×106 | 9.76×10-1 | 1.17×100 |
5 | 2.70×106 | 2.55×106 | 1.06×100 | 1.94×106 | 2.10×106 | 9.26×10-1 | 1.14×100 |
6 | 2.55×106 | 2.53×106 | 1.01×100 | 1.97×106 | 2.10×106 | 9.38×10-1 | 1.07×100 |
RSD | 7.53×100 |
样本号 | 加入基质后 百草枯峰面积 | 溶液中百草枯峰面积 | 百草枯 基质因子 | 加入基质后 内标峰面积 | 溶液中内标 峰面积 | 内标 基质因子 | 内标归一化的基质因子 |
---|---|---|---|---|---|---|---|
低浓度 | |||||||
1 | 1.87×104 | 6.07×102 | 3.09×101 | 1.68×106 | 8.08×105 | 2.08×100 | 1.49×101 |
2 | 2.32×104 | 5.26×102 | 4.40×101 | 1.80×106 | 5.34×105 | 3.38×100 | 1.30×101 |
3 | 2.56×104 | 4.97×102 | 5.16×101 | 1.87×106 | 6.73×105 | 2.78×100 | 1.86×101 |
4 | 2.48×104 | 4.64×102 | 5.33×101 | 1.90×106 | 6.36×105 | 2.98×100 | 1.79×101 |
5 | 2.58×104 | 5.66×102 | 4.56×101 | 1.95×106 | 7.64×105 | 2.56×100 | 1.78×101 |
6 | 7.16×103 | 3.21×102 | 2.23×101 | 9.06×105 | 6.25×105 | 1.45×100 | 1.54×101 |
RSD | 1.33×101 | ||||||
高浓度 | |||||||
1 | 2.11×106 | 2.26×106 | 9.36×10-1 | 1.88×106 | 2.00×106 | 9.43×10-1 | 9.92×10-1 |
2 | 2.51×106 | 2.26×106 | 1.11×100 | 1.85×106 | 2.01×106 | 9.18×10-1 | 1.21×100 |
3 | 4.70×106 | 2.85×106 | 1.65×10-1 | 3.50×105 | 2.21×106 | 1.58×10-1 | 1.04×100 |
4 | 2.63×106 | 2.30×106 | 1.14×100 | 1.99×106 | 2.04×106 | 9.76×10-1 | 1.17×100 |
5 | 2.70×106 | 2.55×106 | 1.06×100 | 1.94×106 | 2.10×106 | 9.26×10-1 | 1.14×100 |
6 | 2.55×106 | 2.53×106 | 1.01×100 | 1.97×106 | 2.10×106 | 9.38×10-1 | 1.07×100 |
RSD | 7.53×100 |
样本 | 室温放置 | 冻融 | 2~8 ℃ | -80 ℃ | ||||
---|---|---|---|---|---|---|---|---|
2 h | 8 h | 1 d | 1次 | 2次 | 3次 | 放置1周 | 放置1个月 | |
高浓度 | 111.83 | 118.66 | 114 | 103.91 | 100.74 | 106.57 | 113.18 | 114.54 |
低浓度 | 97.03 | 100.52 | 100.12 | 90.61 | 91.72 | 99.59 | 104.12 | 103.38 |
样本 | 室温放置 | 冻融 | 2~8 ℃ | -80 ℃ | ||||
---|---|---|---|---|---|---|---|---|
2 h | 8 h | 1 d | 1次 | 2次 | 3次 | 放置1周 | 放置1个月 | |
高浓度 | 111.83 | 118.66 | 114 | 103.91 | 100.74 | 106.57 | 113.18 | 114.54 |
低浓度 | 97.03 | 100.52 | 100.12 | 90.61 | 91.72 | 99.59 | 104.12 | 103.38 |
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