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Table 3 Bioanalytical/metabolite studies

From: Ultra-high performance liquid chromatography-MS/MS (UHPLC-MS/MS) in practice: analysis of drugs and pharmaceutical formulations

UPLC (drug) Column Mobile phase system Detector Extraction method Biological or/metabolite studies or pharmaceutical Mode of analysis Ref
Antibiotics agents
Amoxicillin, Ampicillin, cefuroxime, cefazolin, ceftazidime, meropenem, piperacillin, clavulanic acid, and tazobactam BEH C18 Water (A) Acetonitrile (B) both containing 0.1% formic acid
5% solution (B) at 0.5 min to 55% at 4.0 min and column was rinsed with 95% solution (B) for 0.5 min and re-equilibrated to starting conditions for 1 min
Triple-quadrupole PP Biological Gradient [33]
Cefuroxime lysine BEH C18 Acetonitrile: 0.1% formic acid in 10 mM Ammonium Acetate (40:60, v/v). Quadrupole LLE Biological Isocratic [34]
Clarithromycin BEH C18 (A) 50 mM ammonium Acetate solution and (B) Acetonitrile. 0.0 min 50 (A):50(B), 1.5 min 10(A): 90(B), 1.7 min 10(A): 90(B), 1.8 min 50(A):50(B), 2.0 min 50(A):50(B) Triple-quadrupole mass spectrometer LLE Biological Gradient [35]
Indolinone derivative HSS T3 column Water (A) and (B) acetonitrile, both containing 0.1% formic acid 0–0.5 min, (B) 2%;0.5–2 min, (B) 2–100%; 2–2.5 min, (B) 100%; 2.5–2.6 min, (B) 100–2%; 2.6–4 min, (B) 2% Mass detector PP Biological Gradient [36]
Ertapenem Agilent Zorbax Eclipse Plus C18 Water : Acetonitrile (95:5% v/v) both containing 0.1 % formic Acid Triple-quadrupole LLE Biological Gradient [37]
Amikacin, flucloxacillin, meropenem, penicillin G and vancomycin RP18 column Water (A) and methanol (B), both containing 4% of formic acid
0–0.3 min, 20% (B); 0.3–1.0 min, 50% (B); 1.0–2.0 min
50% (B); 2.0–2.7 min, 75% (B), 2.7–5.3 min, 75% (B)
5.3–5.5 min, 20% (B)
Triple-quadrupole mass spectrometer PP Biological Gradient [38]
Cephalomannine BEH C18 0.1% formic acid in water (A) and acetonitrile (B)
0–0.6 min, 20–85% (B); 0.6–1.8 min, 85% (B); 1.8–2.0 min, 80–30% (B)
Triple-quadrupole mass spectrometer PP Biological Gradient [39]
Tedizolid and linezolid BEH C18 (A) 0.1% formic acid in water and (B) Acetonitrile
0–0.3 min, 20–95% (B); 0.3–1.5 min, 95–95% (B); 1.5–1.6 min, 95–20% (B); 1.6–3.0 min, 20–20% (B)
Mass spectrometer PP Biological Gradient [40]
Anticancer agents
Amrubicin BEH C18 (A) Acetonitrile: water, (1:99% v/v), 5 mM formic acid and (B) acetonitrile: water, (99:1% v/v), also containing 5 mM formic acid 0.00 min, 100(A) :0(B); 0.30 min, 0(A):100 (B); 0.70 min, 0(A):100 (B); 1.50 min, 100(A): 0(B) Triple-quadrupole SPE Metabolite Gradient [41]
Solasonine HSS T3 column (A) 0.1% formic acid and (B) acetonitrile. 0–0.5 min, 15% (B); 0.5–3.5 min, 15–75% (B); 3.5–4.0 min, 75–85% (B); 4.0–5.0 min, 85% (B) Triple-quadrupole mass spectrometer PP Biological Gradient [42]
Berberrubine BEH C18 (A) 0.1% formic acid and (B) acetonitrile. 1.5 min, 30–60% (B); within 0.5 min, 95% (B); then decreased to 30% (B) within in 0.1 min, then maintained 30% for 0.4 min Triple-quadrupole mass spectrometer LLE Biological Gradient [43]
Pomalidomide BEH C18 Acetonitrile: 10 mM Ammonium Acetate (80:20% v/v) Triple-quadrupole mass spectrometer LLE Biological Isocratic [44]
Docetaxel BEH C18 (A) Water containing 0.5% formic acid (pH 2.23) and (B) 0.5% formic acid in acetonitrile (pH 2.24). 0–0.9 min, 90% (A); 0.9–1.6 min, 100% (B); 1.6–1.7 min, 90% (A), 1.7–2.5 min, 90% (A) Quadrupole LLE Biological Gradient [45]
Indolinone derivative HSS T3 column Water (A) and (B) acetonitrile, both containing 0.1% formic acid. 0–0.5 min, 2% (B); 0.5–2 min, 2–100% (B); 2–2.5 min, 100% (B); 2.5–2.6 min, 100–2% (B); 2.6–4 min, 2% (B) Mass detector PP Biological Gradient [36]
Lenalidomide BEH C18 Acetonitrile: water: formic acid (65:35:0.1% v/v/v) Triple-quadrupole mass spectrometer PP Biological Isocratic [46]
Paclitaxel BEH C18 Methanol–0.1% aqueous formic acid
(75: 25% v/v)
Triple-quadrupole mass spectrometer LLE Biological Isocratic [47]
Irinotecan and 7-ethyl-10 hydroxycamptothecin (SN-38) BEH C18 (A) Ammonium acetate Buffer (10 mM; pH 3.5) with 0.1% formic acid and (B) acetonitrile. 0 min, 20% (B); 3 min, 20–70% (B), 0.2 min, 70–98% (B), 0.7 min 98% (B); 0.2 min, 98–20% (B) Quadrupole SPE Biological Gradient [48]
Anticancer c-Met
inhibitor LS-177
C18 column (A) Acetonitrile and (B) 0.1% formic acid in water. 0 min, 20% (A); 1 min, 80% (A); 2 min, 80% (A); 2.5 min, 20% (A); 3 min, 20% (A) Triple-quadrupole mass spectrometer LLE Biological Gradient [49]
TM-2 C18 column (A) Acetonitrile and (B) 2 mmol/L ammonium acetate in water. 1.5 min, 60–90% (A); 2.8 min, 90% (A); 3.5 min, 90–60% (A) Triple-quadrupole mass spectrometer LLE Biological Gradient [50]
Methotrexate polyglutamates BEH C18 (A) 10 mM Ammonium bicarbonate buffer With 5 mM of the desired ion-pair adjusted to pH 7.5 with formic acid and (B) acetonitrile. 1 min, 90% (A); 9 min, 70% (A): 30% (B) Triple-quadrupole mass spectrometer PP Biological Gradient [51]
Ciprofloxacin, cyclophosphamid, tamoxifen, and azathioprine HSS T3 (A) 0.1 % formic acid (A) and (B) acetonitrile. 0 min, 90% (A) and 5% (B); 10 min, 0% (A) and 100 % (B) Triple-quadrupole mass spectrometer SPE Pharmaceutical Gradient [52]
Temozolomide BEH C18 (A) Water (containing 0.1% formic acid and 10 mM ammonium acetate) and (B) acetonitrile. 0 min, 20% (B); 2 min, 20–50% (B); 1 min, 50% (B); 1 min, 50–20% (B) Quadrupole mass spectrometer PP Biological Gradient [53]
Dendrobine BEH C18 (A) 0.1% formic acid and (B) acetonitrile. 0–1.0 min, 20–40 (B); 2 min, 40–95% (B), 0.5 min, 95% (B); then decreased to 20% (B) within 0.1 min, maintained at 20% (B) for 0.4 min Triple-quadrupole mass spectrometer PP Biological Gradient [54]
Simotinib Zorbax SB-C8 column 0.1 % formic Acid with 10 mM ammonium formate: methanol (20:80% v/v) Mass detector LLE Biological Isocratic [55]
Nintedanib BEH C18 (A) acetonitrile and (B) 0.1% formic acid in water
0–0.3 min, 20–95% (A); 0.3–2.0 min, 95–95% (A); 2.0–2.1 min, 95–20% (A); 2.1–3.0 min, 20–20% (A)
Triple-quadrupole mass spectrometer PP Metabolite Gradient [56]
Letrozole C18 column (A) Acetonitrile and 0.1% formic acid in water (B). 0 min, 20% (A): 80% (B); 0.3 min, 20% (A): 80% (B); 2 min, 95% (A): 5% (B); 2.5 min, 95% (A): 5% (B); 2.6 min, 20 % (A): 80% (B) Triple-quadrupole mass spectrometer PP Biological Gradient [57]
Parthenolide BEH C18 (A) Acetonitrile and 0.1% formic acid in water (B). 0–0.3 min, 20–95% (B); 0.3–1.5 min, 95–95% (B), 1.5–1.6 min, 95–20% (B) Triple-quadrupole mass spectrometer SPE Biological Gradient [58]
Tamoxifen BEH C18 (A) 10 mM Ammonium formate in water and acetonitrile (B) both are containing 0.1%formic acid
0.0 min, 70%(A): 30%(B); 9.0 min, 48% (A): 52%(B); 9.01 min, 48% (A): 52%(B); 9.50 min, 70% (A): 30%(B); 13 min 70% (A): 30%(B)
Triple-quadrupole mass spectrometer PP Metabolite Gradient [59]
Vincristine HSS T3 column (A) Methanol and (B) water containing 0.2% formic acid. 3 min, 30–95% (A); and returned to initial condition within 1 min Triple-quadrupole mass spectrometer LLE Biological Gradient [60]
Palonosetron HSS T3 column Methanol : water containing 0.1% formic acid 80: 20% v/v Triple-quadrupole LLE Biological Isocratic [61]
Kurarinone BEH C18 (A) Acetonitrile and 0.1% formic acid in water (B)
0–0.3 min, 30–30% (A); 0.3–1.0 min, 30–90% (A); 1.0–2.0 min, 90–90% (A); 2.0–2.1 min, 90–30% (A); 2.1–3.0 min, 30–30% (A)
Triple-quadrupole LLE Biological Gradient [62]
Antiviral agents
Elbasvir BEH C18 (A) Acetonitrile and water (containing 5.0 mM ammonium acetate with 0.01% acetic acid, pH 4.5) (B)
0.0–0.5 min, 90–90% (A)
0.5–1.2 min, 90–5% (A); 1.2–2.0 min, 5–5% (A); 2.0–2.2 min, 5–90% (A); 2.2–3.0 min, 90–90% (A)
Triple-quadrupole PP Biological Gradient [63]
Daclatasvir HSS C18 10 mM Ammonium formate, pH 3.5 and acetonitrile (50:50% v/v) Quadrupole LLE Biological Isocratic [64]
Ribavirin, sofosbuvir BEH C18 (A) Acetonitrile and 0.1% formic acid in water (B)
0–0.5 min, 10–10% (A); 0.5–1.0 min, 10–95% (A); 1.0–2.0 min, 95–95% (A); 2.0–2.1 min, 95–10% (A); 2.1–3.0 min, 10–10% (A)
Triple-quadrupole mass spectrometer PP Metabolite Gradient [65]
Atazanavir, Darunavir and Ritonavir C18 column (A) 10 mM Ammonium Formate, pH 4.0, adjusted with formic acid in water, and acetonitrile (B). 0.0–0.8 min, 50%(A) and 50%(B); 0.8–1.2 min, 30%(A) and 70%(B) Mass detector PP Biological Gradient [66]
Oleanolic acid C18 column 10 mM Ammonium Acetate with 0.1% formic acid in water: acetonitrile (10: 90% v/v) Triple-quadrupole mass spectrometer SPE Biological Isocratic [67]
Antifungal agent
Tizoxanide BEH C18 Aq. ammonium formate buffer 10 mM, adjusted to pH 3.0 with formic acid, and acetonitrile (40: 60% v/v) Mass detector LLE Biological Isocratic [68]
Voriconazole BEH C18 Acetonitrile and water containing 1% formic acid (45: 55% v/v) Triple-quadrupole mass spectrometer LLE Biological Isocratic [69]
Amphotericin B BEH Shield RP18 column (A) Methanol: acetonitrile (50 : 50% v/v) containing 0.1% formic acid; and (B) 10 mM ammonium formate (pH 3 ± 0.2), containing 0.2% formic acid and 1% acetonitrile
0.0–2.0 min, 35–90% (A); 2.0–2.7 min, 90–35% (A)
Triple-quadrupole mass spectrometer SPE Biological Gradient [70]
Fluconazole, Itraconazole, Hydroxyitraconazole, Posaconazole, Voriconazole C18 column (A) 10 mM Ammonium formate in ultrapure water with 0.1% formic acid and acetonitrile with 0.1% formic acid (B) Triple-quadrupole mass spectrometer PP Biological Isocratic [71]
Posaconazole BEH C18 (A) 10 mM Ammonium formate in water containing 0.1% formic acid, (B) 1% acetic acid in methanol, and (C) 1% acetic Acid in acetonitrile. 0–0.9 min, 90% (A) and 10% (B); 0.9–1.9 min, 5% (A) and 95% (B); 1.9–2 min, 100% (B); 2–3.6 min. 100% (C); 3.6–3.7 min, 90% (A) and 10% (B); 3.7–5.0 min, 90% (A) and 10% (B) Triple-quadrupole mass spectrometer PP Biological Gradient [72]
Cardiovascular agents
Atorvastatin, Ezetimibe BEH C18 (A) 0.1% Formic acid in water : (B) acetonitrile (95: 5% v/v)
0.0–0.4 min, 95% (A) and 5%(B); 0.4–1.1 min 10 %(A) and 90% (B); 1.1 min, 95% (A) and 5% (B)
Triple-quadrupole LLE Biological Gradient [73]
4-hydroxyphenyl carvedilol BEH C18 Acetonitrile- 4.0 mM ammonium formate, pH 3.0 adjusted with 0.1% formic acid (78: 22% v/v) Triple-quadrupole mass spectrometer SPE Metabolite Isocratic [74]
Ivabradine, Reboxetine, Metoprolol BEH C18 (A) Water and (B) methanol, both containing 2 mM ammonium acetate.0.0–0.5 min, 20% (B); 0.5–3.0 min, 20–90% (B); 3.0–3.5 min, 90% (B) 3.5–4.5 min, 20% (B) Quadrupole mass spectrometer LLE Biological Gradient [75]
Meldonium BEH HILIC column Water: acetonitrile: formic acid (adjusted to pH 3.0 with 12.5% ammonia hydroxide) (25: 70: 5% v/v/v) Triple-quadrupole mass spectrometer PP Biological Isocratic [76]
Candesartan, Hydrochlorthiazide C18 Phenomenex Methanol : Acetonitrile 1 (15: 85% v/v) Triple-quadrupole mass spectrometer LLE Biological Isocratic [77]
Doxazosine BEH C18 (A) and (B) consisted of 0.05 (w/v) pentadecafluorooctanoic acid in acetonitrile and 0.05 (w/v) pentadecafluorooctanoic acid in water. 1.0–1.45 min, 10–99% (A); 1.45–1.55 min, 99–10% (A); 1.55–2.0 min, 10% (A) Triple-quadrupole mass spectrometer LLE Biological Gradient [78]
Lercanidipine BEH C18 70% Acetonitrile in water containing 0.2% v/v formic acid Triple-quadrupole mass spectrometer LLE Biological Isocratic [79]
Aliskiren Hemifumarate, Amlodipine Besylate and Hydrochlorothiazide BEH C18 0.1% Formic acid in ammonium acetate buffer (0.02 M, pH 3.5) and Methanol
(25: 75% v/v)
Triple-quadrupole mass spectrometer LLE Biological Isocratic [80]
Irbesartan BEH C18 Acetonitrile: Methanol: 10 mM Ammonium acetate (70:15: 15% v/v/v) Triple-quadrupole SPE Biological Isocratic [81]
Amlodipine, benazeprile and benazeprilat BEH C18 (A) 0.1% Formic acid and Acetonitrile (B)
0–0.2 min, 95% (A) and 5% (B); 0.2–0.3 min, 0%(A) and 100%(B); 0.3–2.0 min, 0%(A) and 100%(B); 2.0–2.5 min, 95% (A) and 5% (B), 2.5 min, 95% (A) and 5% (B)
Triple-quadrupole mass spectrometer LLE Biological Gradient [82]
Candesartan Betasil C8 column Methanol : ammonium tri-floro acetate buffer with formic acid (60: 40% v/v) Mass detector PP Biological Isocratic [83]
N-butylscopolamine C18 column Acetonitrile: 5 mM ammonium acetate: 0.1% formic acid (90: 10% v/v) Triple-quadrupole mass spectrometer SPE Biological Isocratic [84]
Udenafil BEH C18 Acetonitrile: 0.1% formic acid
(75: 25% v/v)
Quadrupole mass spectrometer LLE Metabolite Isocratic [85]
Alprostadil BEH C18 (A) Acetonitrile and water (B), containing 0.1% formic acid
0.0–0.6 min, 30% (A); 0.6–0.8 min, 60% (A); 1.4 min, 30% (A)
Quadrupole mass Spectrometer LLE Biological Gradient [86]
Analgesic agents
Sumatriptan Hypersil gold C18 Methanol:water (90:10% v/v) Mass detector PP Biological Isocratic [87]
Sufentanil BEH C18 Acetonitrile : water (4:55% v/v) Triple-quadrupole mass spectrometer SPE Biological Isocratic [88]
Mitragynine BEH HILIC column 10 mM Ammonium formate buffer containing 0.1% formic acid: acetonitrile (15:85% v/v) Quadrupole LLE Biological Isocratic [89]
Tapentadol and tapentadol-O-glucuronide BEH C18 0.01 M Ammonium formate (adjusted to pH 4 using formic acid) (A) and methanol (B). For Tapentadol-0.00 min, 80% (A):20%(B); 0.85 min, 65%(A):35%(B); 0.90 min, 2%(A):98% (B); 1.25 min, 2%(A):98% (B); 1.30 min, 80% (A): 20%(B); 1.60 min, 80% (A): 20%(B)
Tapentadol-O-glucuronide-0.0 min, 80% (A): 20%(B); 0.50 min, 70% (A): 30%(B); 0.55 min, 2% (A): 98%(B); 1.05 min, 2% (A): 98%(B); 1.10 min, 80% (A): 20%(B); 1.50 min, 80% (A): 20%(B)
Triple-quadrupole mass spectrometer SPE Biological Gradient [90]
Dexmedetomidine BEH C18 0.1% Formic acid in water (A) and 0.1% formic acid in acetonitrile (B). 0 min, 25%(B); 3.0 min, 25%(B); 3.1 min, 95%(B); 5.0 min, 95%(B); 8.0 min, 2%(B) Triple-quadrupole mass spectrometer SPE Biological Gradient [91]
Nalbuphine BEH HILIC column Acetonitrile : water (83:17% v/v) that contained 0.2% formic acid and 4 mM ammonium formate Triple quadrupole mass spectrometer LLE Biological Isocratic [92]
Buprenorphine and norbuprenorphine BEH C18 Ammonium formate buffer 20 mM adjusted to pH 3.05 with formic acid (A) and acetonitrile (B) (90:10% v/v)
0.0 min, 10 % (B); 2.5 min, 25% (B); 3.2 min, 25% (B); 5.0 min. 30% (B)
Quadrupole mass spectrometer PP Biological Gradient [93]
Anti-steroid
Testosterone and 5-dihydrotestosterone BEH C18 (A) Water, (B) consisted of 2 mM ammonium acetate (native pH) in acetonitrile: water (98:2% v/v)
0.1 min, 0% (B); 1.0 min, 30% (B); 2.0 min, 32% (B); 3.4 min, 32% (B)
Triple-quadrupole LLE Biological Gradient [94]
Triamcinolone acetonide palmitate and triamcinolone acetonide Phenomenex Luna C18 column (A) Acetonitrile and (B) 0.1% ammonia solution. 0–1.3 min, 34% (A); 1.3–1.5 min, 34–95%(A); 1.5–5.0 min, 95% (A); 5.0–5.2 min, 95–34% (A); 5.2–5.5 min, 34% (A) Triple-quadrupole mass spectrometer LLE Biological Gradient [95]
Anti-inflammatory (NSAID)
Hesperetin Chiralpak IA-3 (A) Water with 0.1% CHOOH and (B) acetonitrile with 0.1% CHOOH. 0 min, 33% (B); 0.5 min 33% (B); 5 min 40% (B); 5.1 min, 100% (B); 6 min, 100% (B); 6.1 min 33% (B); 8 min 33% (B) Triple-quadrupole SPE Biological Gradient [96]
Epiafzelechin a flavan-3-ol with osteoprotective BEH C18 Water (A) and acetonitrile (B) both containing (0.1% Formic Acid v/v) 1–11 min, 0–70% (B); 0–1 min, 100 % (A); 11–16 min, 100% (A) Triple-quadrupole mass spectrometer LLE Biological Gradient [97]
E6005, Phosphodiesterase 4 inhibitor BEH C18 (A) Water: acetonitrile: 1 mol/L ammonium formate (950:50: 5% v/v/v) and (B) water: acetonitrile: 1 mol/L ammonium formate (100:900: 5% v/v/v). Gradient-2.0 min, 5–95% (B); Isocratic- 2.0 min, 95% (B); 1.5 min, 5% (B) Triple-quadrupole mass spectrometer SPE Metabolite Gradient/Isocratic [98]
Naringin BEH C18 Acetonitrile-0.4% acetic acid (80: 20% v/v) Triple-quadrupole mass spectrometer LLE Biological Isocratic [99]
Ibuprofen BEH C18 Water: methanol (35:65% v/v) both containing 10 mM ammonium acetate and 0.1% formic acid. 0–12 min, 35% (A) and 65% (B); 12.01–14 min 100% (B); 15.1 min, 35% (A) and 65% (B) Triple-quadrupole mass spectrometer LLE Biological Gradient [100]
Avicularin BEH C18 0.1% Formic acid in water (A) and (B) acetonitrile. 0–0.50 min, 30–80% (B); 0.50–1.40 min, 80 % (B); 1.40–1.60 min, 80–30% (B) Triple-quadrupole mass spectrometer PP Biological Gradient [101]
Hupehenine BEH C18 0.1% Formic acid (A) and Acetonitrile (B) 0.0–2.0 min, 40–90 % (B); maintained for 0.5 min, 90%(B); 90–40% (B) within 0.1 min and then maintained 0.4 min, for 40% (B) Triple-quadrupole mass spectrometer LLE Biological Gradient [102]
Picfeltarraenins IA and IB C18 column Methanol:water (70 : 30% v/v) Mass detector PP Biological Isocratic [103]
Diclofenac sodium BEH C18 Acetonitrile–0.1% ammonium hydroxide aqueous solution (20:80% v/v). 0.0 min, 20% (A); 0.6–1.5 min, 50% (A); 1.6–2.0 min, 20% (A) Triple-quadrupole mass spectrometer LLE Biological Gradient [104]
21-hydroxy deflazacort BEH C18 Acetonitrile and 4.0 mM ammonium formate, pH 3.5 (90:10% v/v) Triple-quadrupole mass spectrometer SPE Biological Isocratic [105]
Acetaminophen and dihydrocodeine BEH C18 (A) 0.1% formic acid in water and (B) Acetonitrile
0–0.3 min, 50–95% (B); 0.3–0.9 min, 95–95% (B); 0.9–1.0 min, 95–50% (B)
Triple-quadrupole mass spectrometer PP Biological Gradient [106]
Anti-diabetes
Glipizide BEH C18 (A) Acetonitrile and water containing 1% formic acid (B). 0.0 min, 30 % (A):70%(B); 0.3 min, 75% (A)25% (B); 0.7 min, 75% (A) 25% (B); 1.0 min, 30% (A): 70% (B) Triple-quadrupole mass spectrometer SPE Biological Gradient [107]
Lysophosphatidylcholine BEH C18 (A) 0.1% Formic acid in water, (B) 0.1% formic acid in acetonitrile. 0 min, 100% (A); 37 min, 100% (B) Mass detector PP Metabolite Gradient [108]
Miglitol C18 inertsil column Acetonitrile and 2 mM Ammonium Acetate (pH 3.5, 80: 20% v/v) Triple-quadrupole mass spectrometer LLE Biological Isocratic [109]
Exenatide C18 column 0.2% Formic acid (A) and methanol (B)
1.5 min, 10% (B); 1.0 min, 10–90% (B); 0.5 min, 90% (B) a linear decrease from 90–10% (B) in 0.1 min
Mass detector SPE Biological Gradient [110]
Anti-depressant
Vortioxetine BEH C18 0.1% Formic acid in water (A) and acetonitrile (B). 0–0.5 min, 20–95% (A); 0.5–1.9 min, 95–95% (A); 1.9–2.0 min, 95–20% (A); 2.0–3.0 min, 20–20% (A) Triple-quadrupole mass spectrometer PP Biological Gradient [111]
Bupropion BEH Phenyl column (A) Ammonium formate buffer (2 mM, pH 4.0) and (B) acetonitrile. 3.5 min, 95% (A); 4.2 min, 70% (A); 4.7 min, 68.5% (A); 4.8 min, 5% (A)
5.7 min, 95% (A)
Triple-quadrupole mass spectrometer SPE Metabolite Gradient [112]
Venlafaxine and O-desmethylvenlafaxine BEH C18 10 mmol/L Ammonium acetate and methanol (85: 15% v/v) Triple-quadrupole SPE Biological Isocratic [113]
Paroxetine Hypersil Gold C18 column Acetonitrile and 0.1% Glacial acetic acid
(50: 50% v/v)
Triple-quadrupole mass spectrometer LLE Biological Isocratic [114]
Antiepileptic agents
Carbamazepine, carbamazepine-10,11-epoxide, gabapentin, lamotrigine, levetiracetam BEH Phenyl column 5 mM Ammonium bicarbonate buffer pH 7.9 (A) and methanol (B)
0.00 min, 97.5% (A): 2.5%(B); 1.00 min, 95.0% (A): 5.0% (B); 2.00 min, 0.0% (A): 30.0% (B); 3.60 min, 50.0% (A): 50.0% (B); 4.00 min, 50.0% (A): 50.0% (B); 4.30 min, 20.0% (A): 80.0% (B); 4.75 min, 20.0% (A) 80.0% (B); 4.85 min, 97.5% (A): 2.5% (B)
Triple-quadrupole mass spectrometer PP Biological Gradient [115]
Haloperidol, olanzapine, quetiapine, fluoxetine, paroxetine, bromazepam, lorazepam, risperidone and benzodiazepines HSS T3 Acetonitrile (A) and 0.1% formic acid in water (B) 0–1 min, 75% (B); 1–6 min, 75–40%(B); 6 min, 75% (B) Triple-quadrupole mass spectrometer SPE Biological Gradient [116]
Oxcarbazepine BEH C18 Acetonitrile–10 mM ammonium acetate (85:15% v/v) Triple-quadrupole mass spectrometer SPE Biological Isocratic [117]
Benzodiazepine 21 BEH C18 0.1% Formic acid in water (A) and 0.1% formic acid in Methanol (B). 70% A–30% B, ramping to 65%
B over 2.5 min, 70% B over 0.75 min, 77% B over 0.75 min, then to 95% B over 0.05 min and holding at 95% B for 1 min, returning to 30% B and re-equilibrating for 2 min
Mass detector LLE Biological Gradient [118]
Aripiprazole Agilent Eclipse Plus C18 (A) 0.1% Formic acid aqueous and (B) acetonitrile. 0–1.2 min, 10–40% (B); 1.2–1.6 min, 40–100% (B); 1.6–1.9 min, 100% (B); 1.91–2.0 min, 10% (B) Mass detector SPE Biological Gradient [119]
CNS
Levodopa, Carbidopa BEH C18 (A) 5 mM Ammonium formate/formic acid at 1000/1 (v/v) and (B) acetone. 0.2 min, 25% (B); 0.2–1.8 min, 25–50% (B); 90% (B) for 0.9 min Triple-quadrupole and electro chemical PP Biological Gradient [120]
Acetylcholine, histamine (HA) BEH HILIC column (A) 0.2% Formic acid and 20 mM ammonium formate in Water (B) acetonitrile. 0 min, 90% (B); 0–1.25 min, 10–70% (B) Triple-quadrupole mass spectrometer PP Metabolite Gradient [121]
Proton pump inhibitor
Esomeprazole, Rabeprazole and Levosulpiride Hypersil gold C18 (A) 2 mM Ammonium formate in water and (B) acetonitrile. 0.01 min, 10% (B); 0.20 min, 10% (B); 0.50 min, 90% (B); 0.70 min, 90% (B); 0.80 min, 10% (B); 1.00 min, 10% (B) Triple-quadrupole mass spectrometer LLE Biological Gradient [122]
Anti-tubercular
Ethambutol, isoniazid and rifampicin HSS T3 Water: methanol (50: 50% v/v) Quadrupole PP Biological Isocratic [123]
Vitamin
Thiamin, riboflavin, Flavin, adenine dinucleotide, nicotinamide, and pyridoxal HSS T3 10 mM Ammonium formate (A) and acetonitrile (B). 0 min, 95% (A); 1 min, 65% (A); 2 min, 45% (A); 2.1–3 min, 5%
(A), 3.1–4 min, 95% (A)
Mass detector LLE Biological Gradient [124]
Uracil and dihydrouracil HSS T3 column (A) 0.1% (v/v) Formic acid in UPLC-grade water and (B) 0.1% (v/v) formic acid in UPLC-grade acetonitrile. 0–.0 min, 0% (B); 3.0–3.2 min, 0–90% (B); 3.2–3.7 min, 90% (B); 3.7–5 min, 0% (B) Triple-quadrupole mass spectrometer LLE Biological Gradient [125]
Immunosuppressant
Tacrolimus BEH C18 10 mM Ammonium acetate, pH 6.00, adjusted with Formic acid and methanol (5:95% v/v) Triple quadrupole mass spectrometer SPE Biological Isocratic [126]
Typhaneoside and Isorhamnetin-3-O-Neohesperidoside BEH C18 (A) Acetonitrile and water (containing 0.1% formic acid) (B) 0 min, 80% (A); 1.7 min, 68% (A); 3.2 min 30% (A); 4.0 min, 20% (A) Mass detector Pollen typhae extract Biological Gradient [127]
Mycophenolic acid BEH C18 Acetonitrile and 10 mM Ammonium formate, pH 3.0 (75:25% v/v) Mass detector PP Biological Isocratic [128]
Anticoagulant
Warfarin BEH C18 (A) 0.2% Formic acid and 1% acetonitrile in water; and (B) 0.2% formic acid in acetonitrile. 80–70% (A) in 1.5 min and then changed linearly to 35% A for another 1.5 min, and remained for a further 0.8 min before changing back to 80% (A) Mass detector PP Biological Gradient [129]
Clopidogrel BEH C18 Acetonitrile and water containing 0.15% formic acid (75: 25% v/v) Triple-quadrupole mass spectrometer LLE Biological Isocratic [130]
Expectorant
Hupehenine BEH C18 (A) 0.1% Formic acid and acetonitrile (B). 0–2.0 min, 40–90% (B); maintained for 90% (B) for 0.5 min, then decreased to 40% within 0.1 min, then maintained at 40% for 0.4 min Triple-quadrupole mass spectrometer LLE Biological Gradient [102]
Multicomponent analysis of drug
Gestodene, Ethinyl estradiol BEH C18 Water (A) and acetonitrile (B) (both containing 0.1% formic acid). 1.5 min, 70% (B); 70–98% (B) within 1.1 min and returned to 70% (B) Quadrupole LLE Biological Gradient [131]
Liensinine, Isoliensinine, and Neferine BEH C18 (A) Water with 0.1 formic acid and acetonitrile (B). 0–1.0 min, 15–90% (B); 1.0–1.8 min, 90% (B); 1.8–2.0 min, 90–15% (B) Triple-quadrupole mass spectrometer PP Biological Gradient [132]
Pinaverium Bromide BEH C18 Acetonitrile: 5 mM ammonium formate (80:20% v/v) Triple-quadrupole mass spectrometer PP Biological Isocratic [133]
Pimpinellin, Isopimpinellin and Phellopterin BEH C18 Methanol: ammonium acetate (65:35% v/v) Triple-quadrupole mass spectrometer LLE Biological Isocratic [134]
Endocannabinoids
2-arachidonoyl glycerol (2AG), 1-arachidonoyl glycerol (1AG), and anandamide
BEH C18 (A) Water contained 2 mM ammonium acetate and (B) methanol and contained 2 mM ammonium acetate. 0.0–0.5 min, 75% (B); 0.5–5.0 min, 79% (B); 5.0–5.5 min, 90% (B); 5.5–6.5 min, 75% (B) Tandem mass spectrometry PP Biological Gradient [135]
Paeoniflorin, albiflorin, ferulic acid, tetrahydropalmatine, protopine, typhaneoside, senkyunolide I BEH C18 (A) 0.1% Formic acid and (B) acetonitrile. 0–1 min, 5–10% (B); 1–6 min, 10–30% (B); 6–7 min, 30–40% (B); 7–8 min, 40–95% (B); 8–10 min, 95–5% (B) Triple-quadrupole mass spectrometer PP Biological Gradient [136]
Caffeine, Tolbutamide, Metoprolol, Dapsone BEH HILIC C18 Acetonitrile: water containing 0.1% formic acid (15:85% v/v) Triple-quadrupole mass spectrometer LLE Biological Isocrati [137]
Xylazine, Free Morphine, Codeine, 6 Acetylmorphine, Cocaine, Benzoylecgonine in Postmortem HSS T3 0.1% Formic acid in water (A) and acetonitrile (B). 0 min, 90% (A): 10% (B); 0.48 min, 90% (A): 10% (B); 0.50 min, 100% (A): 0% (B); 0.60 min, 85% (A): 15% (B); 2.0 min, 66% (A): 34% (B); 2.10 min, 5% (A): 95% (B); 2.25 min, 90% (A): 10% (B); 2.50 min, 90% (A): 10%(B) Triple-quadrupole mass spectrometer SPE Biological Gradient [138]
Bupropion, metroprolol, midazolam, phenacetin, omeprazole and tolbutamide BEH C18 Acetonitrile (A) and water (B) (containing 0.1% formic acid)
0.3-1.8 min, 30-60% (A); increasing to 95% over 0.2-0.5 min, then decreased to 30% within 0.1 min, and maintained at 30% for 0.4 min.
Triple-quadrupole mass spectrometer PP Biological Gradient [139]
Ketoconazole and Voriconazole on the Pharmacokinetics of Oxcarbazepine BEH C18 Acetonitrile (A) and water (B) (containing 0.1% formic acid) 0–1 min, 20–80% (A); 1–1.5 min, 80–80% (A), 1.5–2 min 80–95% (A); 2–2.5 min, 95–95% (A); 2.5–2.6 min, 95–20% (A) Triple-quadrupole mass Spectrometer PP Metabolite Gradient [140]
Neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, and geniposide BEH C18 0.2% Acetic acid and methanol. 0–4.50 min, 15–30% (B); 4.50–5.50 min, 30–65% (B); 5.50–6.00 min, 65–15% (B); 6.00–7.50 min, 15–15% (B) Triple-quadrupole mass Spectrometer PP Biological Gradient [141]
Evodiamine and Rutaecarpine BEH C18 Acetonitrile (A) and water (B) both containing 0.2% Formic acid. 0 min, 40% (A): 60% (B); 0–0.6 min, 70% (A): 30% (B); 0.6–1.0 min, 70% (A): 30% (B); then returned to 40% (A):/60% (B) Triple-quadrupole mass Spectrometer LLE Biological Gradient [142]
Bosentan and glimepiride BEH C18 (A) 0.1% Formic acid in water and (B) acetonitrile. 0–0.5 min, 35% (B); 0.5–1.0 min, 35–80% (B); 1.0–1.5 min, 80–35% (B) Triple-quadrupole PP Biological Gradient [143]
Amoxicillin and prednisolone BEH C18 0.1% Formic acid in water (A) and 0.1% formic acid in acetonitrile (B). 0–1 min, 98% (A); 1–1.5 min, 98–15% (A); 1.5–2.5 min, 15% (A); 2.5–3.0 min, 15–2% (A); 3.0–3.5 min, 2–98% (A); 3.5–5.5 min, 98% (A) Triple-quadrupole mass Spectrometer SPE Biological Gradient [144]
Fenofibric acid and berberine Eclipse XDB C18 column (A) Acetonitrile and (B) water (containing 0.1% formic acid). 0.0 min, 30 % (A): 70% (B); 0.3 min, 30% (A): 70% (B); 0.5 min, 50% (A): 50% (B); 1.0 min, 90% (A): 10% (B); 2.5 min, 90% (A): 10% (B); 2.6 min, 30% (A): 70% (B); 3.0 min, 30% (A): 70% (B) Triple-quadrupole mass Spectrometer LLE Biological Gradient [145]