Table 1.
Internal standard | LLE: pH modifier; solvent | Sample volume | Analytical method | LC run time (min) | Linear range (ng/mL) | Recovery (%) | LLOQ | |
---|---|---|---|---|---|---|---|---|
Assay reported | d9-Finasteride | NH4OH; MTBE | 100 μL | LC–MS/MS | 6 | 0.2–50 | 107.4% | 2 pg |
[7] | ±-5-[2-[[2-(o-ethoxyphenoxy)propyl]amino]propyl]-2-methoxybenzenesulphonamide | >1 step incl. S.NaHCO3; EA | 1.5 mL | HPLC | NR (tamsulosin RT 5.9 min) | 0.5–15 | 70% | 525 pg |
[10] | (6)-(R)-5-[3-[[2-(o-ethoxyphenoxy)ethyl] amino]butyl] – 2 – methoxybenzenesulfonamide hydrochloride (AB289) (Yamanouchi) | S. NaHCO3; H:EA | 200 μL | LC–MS/MS | 3 | 0.5–50 | >80% | 25 pg |
[4]a | AB289 (as above) | Details NR | NR | HPLCa | NR | 0.5–50 | NR | NR |
[8] | 1-(2,6-Dimethyl-3-hydroxylphenoxy)-2- (3,4-methoxyphenylethylamino)-propane hydrochloride | S. NaHCO3; EA | 1 mL | LC–MS | 8 | 0.2–30 | 84.2–94.5% | 40 pg |
[6] | Analogue of tamsulosin: (R)-5-[2-[(3-(2-ethoxyphenoxy)propyl)amino]-2-methylethyl]-2-methoxybenzensulfonamide (Léčiva) | Na2CO3; BA | 1 mL | HPLC | 3.5 | 0.4–40 | NR | 360 pg |
[3] | Mosapride | NaOH; DEE:DCM | 100 μL | LC–MS/MS | 2 | 0.1–50 | 59.3% | NR |
[11] | Labetalol | S. NaHCO3; EA | 1 mL | LC–MS/MS | 5 | 0.1–19.3 | 66–77% | 17.5 pg |
[12] | Diphenhydramine hydrochloride | MTBE | 500 μL | LC–MS/MS | 2 | 0.01–20 | 78% | 5 pg |
[9] | Diphenhydramine | NaCO3, H, EA | 200 μL | LC–MS/MS | NR (tamsulosin RT 2.2 min) | 0.1–30 | 73% | 2 pg |
LLE, liquid–liquid extraction; LC, liquid chromatography; MTBE, methyl tert-butyl ether; LC–MS/MS, liquid chromatography tandem mass spectrometry; S., saturated; EA, ethyl acetate; HPLC, high performance liquid chromatography; NR, not reported; H, hexane; BA, butyl acetate; DEE, diethyl ether; DCM, dichloromethane; RT = retention time; LLOQ = lower limit of quantitation (on-column).
This method principally describes a radioreceptor assay, details of which are not included in this table. The analytical method developed, validated and presented here is summarised in the first row for comparison.