Table 2.
Analytical methods for the detection of alkaloids
| Alkaloids | Samples | Sample preparation | LOD | LOQ | Analytical method | References |
|---|---|---|---|---|---|---|
|
Ergot Alkaloid |
Cereals and foods | SPE | 0.17–2.78 μg/kg | LC–MS/MS | Krska et al. (2008) | |
| Rye and wheat | SPE |
0.01–1.0 µg/kg (wheat) 0.01–10 µg/kg (rye) |
UPLC-MS/MS | Kokkonen and Jestoi (2010) | ||
| Beer | U-HPLC-Orbitrap MS | Zachariasova et al. (2010) | ||||
| Rye | SPE | 0.25–1.65 μg/kg | 1.10–6.65 μg/kg | HPLC–FLD | Franzmann et al. (2010) | |
| Rye and rye products | Solid-phase filtration | 0.02–1.10 μg/kg | 0.08v3.30 μg/kg | HPLC–FLD | Muller et al. (2009) | |
| 8.1–22.3 μg/kg | 25.5–66.5 μg/kg | |||||
| Claviceps purpurea | GC–MS | Jegorov et al. (1997) | ||||
| Sorghum ergot | 0.01 mg/kg | 0.1 mg | ELISA | Molloy et al. (2003) | ||
| Grasses | ELISA | Tunali et al. (2000) | ||||
| Straw, Seed Digesta | 1.5625 ng/mL | ELISA | Schnitzius et al. (2001 | |||
| Glycoalkaloids | Tomato | 0.39 μg | HPLC–UV | Kozukue et al. (2004) | ||
| 0.94 μg | ||||||
| Potatoes | SPE; C-18 cartridge | RP-HPLC | Houben and Brunt (1994) | |||
| Blood | SPE | 1 μg/L | 2 μg/L | UHPLC-MS/MS | Nara et al. (2019) | |
| Milk | LLE | 0.28 mg/L | GC-NPD | Bushway et al. (1984) | ||
| Potato and tomato | ELISA | Stanker et al. (1994) | ||||
| Potatoes | ELISA | Morgan et al. (1985) | ||||
|
Purine Alkaloids |
Tea, Coffee and Urine | Filtration | 0.10 μg/mL (caffeine) | 0.33 μg/mL | RP-HPLC/UV | Aragao et al.(2005) |
| 0.07 μg/mL (theobromine) | 0.23 μg/mL | |||||
| 0.06 μg/mL (theophylline) | 0.18 μg/mL | |||||
| Tea | Infusion | 0.07–0.47 mg/L | 0.21–1.41 mg/L | HPLC–DAD | Azevedo et al. (2019) | |
| Tea | 0.025 μg/mL (caffeine) | 0.08 μg/mL | UHPLC-MS | Aqel et al. (2019) | ||
| 0.015 μg/L (theobromine) | 0.05 μg/mL | |||||
| 0.01 μg/mL (theophylline) | 0.03 μg/mL | |||||
| Tea | Leaching | HPLC | Jankech et al. (2019) | |||
| Beverage and Food |
Drop-to-drop solvent microextraction |
4.0 ng/mL | GC–MS | Shrivas and Wu (2007) | ||
| Beverage | Ultrasonication | 0.01 mg/L | GC–MS | Zou and Li (2006) | ||
| Soft drinks, tea and coffee | FTIR | Paradkar and Irudayaraj (2002) | ||||
| Yerba mate |
Cellulose acetate membrane |
1.6 × 10–3 mg/kg | 4.2 × 10–3 mg/kg | NIR | Mazur et al. (2014) | |
| Coffee and tea | Infusion |
UV–Visible spectrophotometry |
Lopez-Martinez et al. (2003) | |||
| Pyrrolizidine Alkaloids | Herbal Medicines |
Mixed mode (MCX) cationic exchange SPE cartridge |
0.03–3.37 μg/kg | LC–ESI–MS/MS | Jeong et al. (2021) | |
| Fodder, hay, silage |
SPE, Strata 60 mg, 3 cc cartridges |
3–10 μg/kg | 10 – 30 μg/kg | UHPLC-MS/MS | Mudder et al. (2009) | |
| Plant, milk and urine | SPE | 0.05–0.2 μg/L (milk) | LC–MS/MS | Hoogenboom et al. (2011) | ||
| 0.2v0.5 μg/g (dried plant) | ||||||
| 0.2–0.5 μg/L (urine) | ||||||
| Honey and herbal tea | SPE | 0.5 μg/kg (honey) | 1 μg/kg (honey) | UHPLC-MS/MS | Reinwaldt et al. (2017) | |
| 2.5–10 μg/kg (herbal tea) | 5–20 μg/kg (herbal tea) | |||||
| Senecio inaequidens | Soxhlet | GC–MS | Caniato et al. (1989) | |||
| Senecio alpinus | Soxhlet | GC–MS | Luthy et al. (1981) | |||
| Senecio jacobaea | Extraction with DCM | GC–MS | Pelser et al. (2005) | |||
| Senecio species | Extraction with H2SO4 | GC–MS | Witte et al. (1992) | |||
| Herbal remedies | SPE | GC–MS | Conradie et al. (2005) | |||
| Petasites hybridus | Extraction with methanol | 0.11–1.53 ng/mL | 0.1 ppm | ELISA | Langer et al. (1996) | |
| Senecionine | 0.5–10 ppb | ELISA | Roseman et al. (1996) | |||
| 5–100 ppb | ||||||
| 600–1000 ppb | ||||||
| Antibodies | ELISA | Zundorf et al. (1998) | ||||
| Quinolizidine Alkaloids | Holstein cattle |
Rotary evaporation, Mechanical rotation, DCM |
HPLC–MS | Green et al. (2015) | ||
|
Lupin flours, Lupin-based ingredients and food |
Soxhlet extraction | 2 mg/kg | GC–MS | Resta et al. (2008) | ||
| Lupin seeds | Soxhlet | 2 mg/kg | GC–MS | Boschin et al. (2008) | ||
|
Lupin seeds and Lupin-containing foods |
Centrifugation, silica cartridge |
1 mg/kg | GC–MS/GC-FID | Reinhard et al. (2006) | ||
| 6 mg/kg | ||||||
| 2 mg/kg | ||||||
| Lupinus Species | Centrifugation | GLC, GC-EIMS | Wink et al. (1995) | |||
|
Tropane Alkaloids |
Plasma | Centrifugation | 0.004–0.01 ng/mL | 0.05–0.8 ng/mL | LCI-ESI–MS/MS | John et al. (2010) |
| Atropine | Water dilution | HPLC–UV/MS | Breton et al. (2005) | |||
|
Feedstuff and Biological Samples |
SPE, C-18 cartridge | 12.05 ng (scopolamine) | 37.98 ng (scopolamine) | RP-HPLC/UV | Papadoyannis et al (1993) | |
| 13.25 ng (hyoscyamine) | 38.17 ng (hyoscyamine) | |||||
| Buckwheat | Soxhlet | 0.3 μg/kg (atropine) | 1 μg/kg (atropine) | GC–MS | Caligiani et al. (2011) | |
| 1.0 μg/kg (scopolamine) | 6 μg/kg (scopolamine) | |||||
| Antibodies | Methanol, DCM | 0.1 ng | ELISA | Fliniaux and Jacquin-Dubreuil. (1987) | ||
| Datura |
28% EtOH/NH4OH (9:1), Centrifugation |
0.15 ng | Radioimmunoassay | Savant and Dougall (1990) |