US EPA

7491461 

Journal Article 

Development and validation of an HPLC-MS/MS method for simultaneous determination of ivermectin, febantel, praziquantel, pyrantel pamoate and related compounds in fixed dose combination for veterinary use 

Pontes, FLD; Pontarolo, R; Campos, FR; Gasparetto, JC; Cardoso, MA; Piantavini, MS; Badarã³, A 

2013 

6 

2 

191-200 

English 

High performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) method for simultaneous quantification of ivermectin, febantel, praziquantel and pyrantel pamoate in addition to the qualitative determination of febantel-related compound C and praziquantel-related compounds A, B and C in tablets was developed and validated. Chromatographic separations were achieved using isocratic elution (200 μL/min) on a C8 column (50 × 2.1 mm i.d) coupled with a C8 (10 × 2.1 mm i.d) guard column maintained at 20 °C. The mobile phase consisted in water/acetonitrile (15:85 v/v) containing 0.1% formic acid and 3 mmol/L ammonium formate. The injection volume used was 20 μL. The validation parameters indicated that the method has high sensitivity and selectivity with excellent linearity (r ≥ 0.99). The observed range of recovery was 93.26% to 101.36% with a RSD of <5% for intraday and interday precision. Sample analyses demonstrated a lack of standardization in the amounts of these drugs, which may contribute to their toxicity or a reduction in efficacy, depending of the sample used. The proposed HPLC-MS/MS method is presented as an alternative option for the quality control of pharmaceutical preparations containing these drugs. 

Febantel; HPLC-MS; Ivermectin; MS; Praziquantel; Pyrantel pamoate; Validation; 1 methyl 2 [2 (thiophen 2 yl)ethenyl] 1,4,5,6 tetrahydropyrimidine; 2 (cyclohexylcarbonyl) 2,3,6,7 tetrahydro 4h pyrazino[2,1 a]isoquinolin 4 one; 2 benzo 1,2,3,6,7,11b hexahydro 4h pyrazin[2,1 a]isoquinolin 4 one; acetonitrile; albendazole; ammonium formate; anthelmintic agent; eprinomectin; febantel; formic acid; ivermectin; methyl [5 (phenylsufanyl) 1h benzimidazol 2 yl]carbamate; n formyl n [2 oxo 2 (1 oxo 3,4 dihydroisoquinolin 2(1h) yl)ethyl]cyclohexanecarboxamide; praziquantel; pyrantel embonate; unclassified drug; accuracy; article; drug determination; drug stability; drug structure; elution; high performance liquid chromatography; limit of detection; limit of quantitation; process development; product recovery; quantitative analysis; sensitivity analysis; separation technique; tablet; tandem mass spectrometry; validation process; veterinary medicine