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Chinese Journal of Clinical Pharmacology and Therapeutics ›› 2007, Vol. 12 ›› Issue (4): 385-391.

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Determination of bencycloquidium bromide, a novel anticholinergic compound,in rat’ s bile, urine and feces by LC-ESI-MS

XU Qin1, DINg/Li1, LIU Wen-ying1, CHEN Xiao-ping2, LI Rong-shan1, SONG Qin-xin1   

  1. 1Department of Pharmaceutical Analysis, China Pharmaceutical University, Nanjing 210009, Jiangsu, China;
    2Beijing Shiqiao Biological and Pharmaceutical Co.Ltd., Haidian Area, Beijing 100080, China
  • Received:2007-03-08 Revised:2007-03-08 Published:2020-10-30

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Abstract: AIM: This study was undertaken to study the excretion rule of bencycloquidium bromide (BCQB) in rats, and a LC-ESI-MS method was developed for the determination of BCQB in bile, urine and feces sample of rats. METHODS: A liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) assay for the determination of BCQB in rats bile, urine and feces was firstly developed and validated.After addition of 1-ethyl-bencycloquidium bromide as an internal standard (I.S.), the biological samples were prepared by using solid phase extraction on a C18-cartridge column.Chromatographic separation was analyzed on a Hanbon Lichrospher 5-C18 column.The mobile phase consisted of methanol-40 mmol L ammonium acetate buffer-formic acid (70:30: 0.3, v v v) was pumped at 0.8 mL min for bile.The mobile phase consisted of methanol-40mmol L ammonium acetate buffer-formic acid (75:25:0.25, v v v) was pumped at 1.0 mL min for urine and feces.LC-ESI-MS was carried out on a single quadrupole mass spectrometer using electrospray ionization (ESI) and positive selectedion monitoring (SIM).Target ions were monitored at [M] + m z 330.2 for BCQB and [M] +m z 344.2 for I. S.. RESULTS: The extraction recoveries of BCQB in bile, urine and feces were upper 77 %.The RSD of intrarun and inter-run precisions were all below 15 %.The calibration curves were linear over the concentration ranges of 30.15-1507.50 ng mL (r =0.9995) for the BCQB in bile, and the low limit of quantitative (LLOQ) was 30.15 ng mL.The calibration curves were linear over the concentration ranges of 3.02-1507.50 ng mL (r = 0.9997) for the BCQB in urine, and the LLOQ was 3.02 ng mL.The calibration curves were linear over the concentration ranges of 3.02-1507.50 ng mL (r =0.9997) for the BCQB in feces, and the LLOQ was 3.02 ng mL. CONCLUSION: The method is specific, accurate, reliable and sensitive.The established method has successfully been applied to study the excretion of BCQB in rats after intranasal administration.

Key words: bencycloquidium bromide, bile, urine, feces, excretion, LC-ESI-MS

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