PA | m/z | RT | R2 | ME (%) |
---|---|---|---|---|
Intermedine | 300.1 | 6.16 | 0.997 | 105.5 |
Lycopsamine | 300.0 | 6.38 | 0.99 | 116.5 |
Jacobine | 352.1 | 6.91 | 0.998 | 119.2 |
Retrorsine | 352.1 | 8.31 | 0.998 | 117.4 |
Heliotrine | 314.1 | 8.63 | 0.998 | 119.9 |
Seneciphylline | 334.1 | 9.33 | 0.998 | 119.2 |
Senecionine | 336.1 | 11.14 | 0.994 | 122.6 |
Echimidine | 398.0 | 13.18 | 0.998 | 117.1 |
Senkirkine | 366.1 | 13.37 | 0.995 | 106.2 |
Lasiocarpine | 412.1 | 15.11 | 0.996 | 107.5 |
Concentration level (μg kg–1) | Concentration level (μg kg–1) | Concentration level (μg kg–1) | |||||||
---|---|---|---|---|---|---|---|---|---|
1 | 10 | 50 | 1 | 10 | 50 | 1 | 10 | 50 | |
PA | Recovery (%) | Repeatability RSD (%) | Reproducibility RSD (%) | ||||||
Intermedine | 80.6 | 84.6 | 96.3 | 14.6 | 6.0 | 5.4 | 17.7 | 16.6 | 10.1 |
Lycopsamine | 108.2 | 97.4 | 100.6 | 11.1 | 9.1 | 2.5 | 16.3 | 9.2 | 7.1 |
Jacobine | 90.7 | 99.3 | 97.5 | 10.9 | 9.7 | 4.5 | 15.2 | 11.5 | 4.9 |
Retrorsine | 98.2 | 105.5 | 98.6 | 13.6 | 5.2 | 7.5 | 16.8 | 7.3 | 8.5 |
Heliotrine | 80.9 | 101.4 | 95.6 | 8.5 | 4.0 | 4.3 | 15.0 | 7.3 | 5.1 |
Seneciphylline | 108.1 | 101.5 | 111.6 | 7.3 | 5.3 | 2.5 | 12.8 | 11.2 | 15.6 |
Senecionine | 87.2 | 106.9 | 102.4 | 7.5 | 7.2 | 2.3 | 10.3 | 11.2 | 7.6 |
Echimidine | 103.9 | 109.4 | 114.5 | 8.1 | 5.6 | 6.6 | 15.2 | 17.0 | 13.0 |
Senkirkine | 88.0 | 104.5 | 100.5 | 9.1 | 2.9 | 4.4 | 11.8 | 9.5 | 5.3 |
Lasiocarpine | 82.2 | 108.9 | 105.6 | 2.9 | 12.4 | 3.1 | 12.1 | 12.5 | 7.9 |
PA | Number of samples | Mean concentration (μg kg–1) | Median (μg kg–1) | Min.-Max content (μg kg–1) |
---|---|---|---|---|
Intermedine | 4 | 4.8 | 1.9 | <LOQ–14.7 |
Lycopsamine | 5 | 9.4 | 3.0 | 1.7–32.9 |
Retrorsine | 4 | 1.1 | 1.2 | < LOQ–1.8 |
Senecionine | 3 | 1.0 | <LOQ | < LOQ–2.9 |
Echimidine | 7 | 3.3 | 3.8 | 1.4–-5.2 |
Solvents | Ratio (v/v) | Recovery (%) |
---|---|---|
EtAc : MeOH : NH4OH | 8 : 2 : 0.2 | 77–93 |
EtAc : MeOH : NH4OH : TEA | 8 : 2 : 0.1 : 0.1 | 84–98 |
EtAc : MeOH : ACN : NH4OH : TEA | 8: 1 : 1 : 0.1 : 0.1 | 79–105 |
EtAc : MeOH : ACN : NH4OH : TEA | 7: 1.5 : 1.5 : 0.1 : 0.1 | 78–92 |
EtAc : MeOH : ACN : NH4OH : TEA | 8 : 1 : 1 : 0.2 : 0.1 | 76–97 |
EtAc : MeOH : ACN : NH4OH : TEA | 3 : 3 : 3 : 0.1 : 0.1 | 61–93 |
MeOH : NH4OH | 11 : 1.5 | 48–110 |