Table 3 Linearities, LODs, LOQs, recoveries, and RSDs obtained by LC–MS/MS analysis method in Farfarae Flos
No. | Pyrrolizidine alkaloids | Range (ng/mL) | Linearity (r2) | LOD (μg/kg) | LOQ (μg/kg) | Recovery (%) mean ± SD, n = 3 | Intra-day RSDb (%) | Inter-day RSD (%), n = 9 | |||
|---|---|---|---|---|---|---|---|---|---|---|---|
Low level | Medium level | High level | |||||||||
1 | Echimidine | 1.0–40 | 0.999 | 0.1 | 0.2 | 76.1 ± 2.8 | 78.8 ± 7.5 | 91.3 ± 3.5 | 18.8 | 11.6 | |
2 | Echimidine N-oxide | 1.0–40 | 0.999 | 1.7 | 5.1 | 94.9 ± 1.6 | 97.6 ± 8.5 | 107.1 ± 1.8 | 0.9 | 2.7 | |
3 | Erucifoline | 0.5–20 | 0.999 | 0.3 | 1.0 | 73.1 ± 5.9 | 78.1 ± 13.0 | 78.7 ± 4.2 | 12.0 | 7.4 | |
4 | Erucifoline N-oxide | 0.5–20 | 0.999 | 0.2 | 0.6 | 84.4 ± 5.9 | 93.9 ± 12.3 | 89.8 ± 5.8 | 3.8 | 3.4 | |
5 | Europine | 0.5–20 | 0.999 | 0.1 | 0.3 | 82.1 ± 3.7 | 77.8 ± 7.5 | 70.8 ± 5.1 | 8.6 | 7.5 | |
6 | Europine N-oxide | 0.5–20 | 0.999 | 0.03 | 0.1 | 92.1 ± 2.5 | 84.9 ± 5.1 | 74.6 ± 11.6 | 7.2 | 7.7 | |
7 | Heliotrine | 0.5 –20 | 0.999 | 0.03 | 0.1 | 88.7 ± 1.4 | 89.3 ± 8.3 | 91.7 ± 2.7 | 8.8 | 4.6 | |
8 | Heliotrine N-oxide | 0.5–20 | 0.999 | 0.1 | 0.3 | 99.3 ± 1.7 | 99.4 ± 8.5 | 105.4 ± 2.9 | 5.1 | 4.8 | |
9 | Intermedine | 0.5–20 | 0.999 | 0.1 | 0.2 | 82.3 ± 2.3 | 83.4 ± 10.0 | 84.5 ± 1.5 | 8.1 | 6.8 | |
10 | Intermedine N-oxide | 0.5 –20 | 0.999 | 0.3 | 0.8 | 95.8 ± 1.6 | 93.5 ± 8.7 | 95.1 ± 3.8 | 1.6 | 1.0 | |
11 | Jacobine | 2.0 –80 | 0.999 | 3.5 | 10.4 | 70.4 ± 3.0 | 73.1 ± 10.5 | 72.0 ± 3.5 | 10.6 | 12.9 | |
12 | Jacobine N-oxide | 0.5–20 | 0.999 | 0.1 | 0.3 | 118.0 ± 1.6 | 117.5 ± 8.0 | 100.9 ± 15.6 | 3.5 | 4.6 | |
13 | Lasiocarpine | 2.0–80 | 0.999 | 0.1 | 0.3 | 88.7 ± 2.4 | 92.6 ± 8.6 | 107.8 ± 4.5 | 14.3 | 10.0 | |
14 | Lasiocarpine N-oxide | 2.0–80 | 0.997 | 8.1 | 24.2 | 108.9 ± 1.8 | 112.5 ± 9.7 | 117.0 ± 3.2 | 6.2 | 8.5 | |
15 | Lycopsamine | 0.5–20 | 0.999 | 0.1 | 0.3 | 82.5 ± 2.1 | 83.0 ± 7.9 | 87.3 ± 0.8 | 14.3 | 6.2 | |
16 | Lycopsamine N-oxide | 1.0–40 | 0.999 | 0.4 | 1.1 | 95.1 ± 3.1 | 98.8 ± 9.8 | 92.8 ± 4.3 | 12.4 | 7.0 | |
17 | Monocrotaline | 0.5–20 | 0.999 | 0.3 | 0.8 | 88.0 ± 3.5 | 85.9 ± 9.2 | 92.6 ± 1.8 | 8.4 | 5.1 | |
18 | Monocrotaline N-oxide | 0.5–20 | 0.999 | 0.2 | 0.6 | 101.0 ± 2.4 | 99.9 ± 10.3 | 100.0 ± 3.3 | 7.2 | 5.6 | |
19 | Retrorsine | 1.0–40 | 0.999 | 3.1 | 9.3 | 79.8 ± 7.7 | 94.7 ± 11.1 | 81.0 ± 5.5 | 20.1 | 10.1 | |
20 | Retrorsine N-oxide | 1.0–40 | 0.999 | 1.5 | 4.4 | 110.1 ± 3.5 | 103.2 ± 10.4 | 102.8 ± 3.6 | 3.8 | 6.6 | |
21 | Senecionine | 2.0–200 | 0.999 | –a | – | 106.6 ± 5.7 | 108.9 ± 4.7 | 111.2 ± 5.4 | 4.8 | 3.7 | |
22 | Senecionine N-oxide | 2.0–200 | 0.999 | – | – | 113.1 ± 1.2 | 116.7 ± 3.9 | 119.0 ± 5.8 | 3.1 | 2.0 | |
23 | Seneciphylline | 0.5–20 | 0.999 | 0.5 | 1.6 | 71.0 ± 3.6 | 76.1 ± 10.2 | 79.3 ± 6.9 | 17.6 | 6.5 | |
24 | Seneciphylline N-oxide | 0.5–20 | 0.999 | 0.5 | 1.6 | 78.6 ± 6.3 | 86.2 ± 14.8 | 82.0 ± 2.1 | 16.9 | 6.3 | |
25 | Senecivernine | 1.0–40 | 0.999 | 3.0 | 9.0 | 74.0 ± 2.8 | 81.6 ± 9.7 | 84.4 ± 7.8 | 17.8 | 7.2 | |
26 | Senecivernine N-oxide | 1.0–40 | 0.999 | 0.8 | 2.3 | 95.3 ± 2.8 | 101.2 ± 10.0 | 112.3 ± 1.9 | 1.6 | 5.0 | |
27 | Senkirkine | 2.0–200 | 0.999 | – | – | 92.8 ± 1.2 | 111.4 ± 12.8 | 114.3 ± 8.7 | 6.8 | 5.1 | |
28 | Trichodesmine | 1.0–40 | 0.999 | 0.3 | 0.9 | 81.8 ± 2.1 | 87.0 ± 7.9 | 94.2 ± 2.8 | 8.0 | 2.5 | |