Quantitative analysis of a quaternary ammonium drug: ipratropium bromide by LC/ESI‐MS<i><sup>n</sup></i> in horse plasma and urine

Garcia, Patrice; Paris, Alice; Leufroy, Axelle; Popot, Marie-Agnès; Bonnaire, Yves

doi:10.1002/bmc.1701

Cited by 3 publications

(3 citation statements)

References 10 publications

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“…In this post‐administration study, CIC was administered to horses via Aservo® EquiHaler® containing an inhalation solution of CIC. The inhalative administration route results in a minor systemic bioavailability and consequently in a very low amount of native molecule (and/or metabolites) in biological fluids requiring highly specific and sensitive analytical methods 38 …”

Section: Resultsmentioning

confidence: 99%

“…The inhalative administration route results in a minor systemic bioavailability and consequently in a very low amount of native molecule (and/or metabolites) in biological fluids requiring highly specific and sensitive analytical methods. 38 The specificity was assessed by analyzing 10 blank plasma samples. No signal was detected at the expected retention times of CIC and des-CIC proving the specificity of the method.…”

Section: Methods Performancesmentioning

confidence: 99%

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LC‐HRMS/MS study of the prodrug ciclesonide and its active metabolite desisobutyryl‐ciclesonide in plasma after an inhalative administration to horses for doping control purposes

Trévisiol¹,

Moulard²,

Kaabia³

et al. 2021

Drug Testing and Analysis

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Ciclesonide (CIC) is the first inhaled highly potent corticosteroid that does not cause any cortisol suppression. It has been developed for the treatment of asthma in human and more recently in equine. CIC is the active compound of Aservo® EquiHaler® (Boehringer Ingelheim Vetmedica GmbH), the pre‐filled inhaler generating a medicated mist based on Soft Mist™ technology. This prodrug is rapidly converted to desisobutyryl‐ciclesonide (des‐CIC), the main pharmacologically active compound. Due to its anti‐inflammatory properties, CIC is prohibited for use in horse competitions. To set up an appropriate control, the determination of detection times and screening limits are required. Therefore, a highly sensitive analytical method based on supported liquid extraction (SLE) combined with liquid chromatography–high resolution tandem mass spectrometry (LC‐HRMS/MS) was developed to detect CIC and its active metabolite des‐CIC in plasma. The lower limit of detection of CIC and des‐CIC was approximately 1 pg/ml in plasma. After a pilot study conducted on a single horse at the recommended dose (eight actuations twice daily corresponding to 5.5 mg/day for the first 5 days, followed by 12 actuations once daily corresponding to 4.1 mg/day in the last 5 days), the same protocol was applied in the main study using six horses. In all horses, CIC and des‐CIC levels were less than 5 and 10 pg/ml, respectively, at 36 h after the end of the administration. The outcome of this risk assessment study should be useful to draw any recommendations for horse competitions.

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Section: Resultsmentioning

confidence: 99%

Section: Methods Performancesmentioning

confidence: 99%

LC‐HRMS/MS study of the prodrug ciclesonide and its active metabolite desisobutyryl‐ciclesonide in plasma after an inhalative administration to horses for doping control purposes

Trévisiol¹,

Moulard²,

Kaabia³

et al. 2021

Drug Testing and Analysis

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“…At this point, the WCX material, with the advantage of easy to be regenerated, might be applied to enrich and obtain higher content of QAs. WCX chromatography has played an important role in the field of separation and purification of samples, such as drug, urine and plasma samples . With WCX, the effectiveness of separation and purification was markedly improved.…”

Section: Introductionmentioning

confidence: 99%

Enrichment and analysis of quaternary alkaloids from Zanthoxylum simulans using weak cation exchange solid‐phase extraction coupled with LC–MS

Fan

Tian

Chen

et al. 2019

Phytochemical Analysis

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Introduction Quaternary alkaloids (QAs) are the major alkaloids in several traditional Chinese medicines, especially in Zanthoxylum simulans. However, few studies on enrichment of QAs from Z. simulans were conducted due to their high polarity and low content. Objective To develop a weak cation exchange (WCX) solid‐phase extraction (SPE) coupled with liquid chromatography mass spectrometry (LC–MS) method to enrich and identify QAs from Z. simulans. Meanwhile, the qualitative and quantitative analyses of QAs were carried out based on the optimum conditions of the method. Methods Fresh stem bark of Z. simulans was extracted with 70% aqueous methanol and enriched by WCX‐SPE. A high‐performance liquid chromatography coupled with tandem mass spectrometry (HPLC–MS/MS) with an electrospray ionisation (ESI) source was used for the qualitative and quantitative analyses of QAs. Results Significant improvements were observed in resolution and abundance of the peaks with WCX‐SPE. The linearity, limit of detection (LOD) and limit of quantification (LOQ) were determined for this analytical method. The linear relationship (A = 338.85C – 187.72, R2 = 0.99) was explored in the range of 0.5 to 312.5 μg/mL for chelerythrine. The LOD and LOQ for chelerythrine standard solutions were 0.0539 μg/mL and 0.1798 μg/mL, respectively. In addition, 22 peaks were detected successfully with WCX‐SPE and nine of them are undetectable without the processing of WCX‐SPE. Conclusion A highly selective and efficient method for simultaneous enrichment and identification of QAs from crude extract of Z. simulans was developed for the first time by combining WCX‐SPE with LC–MS.

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Development and Validation of Stability Indicating Method for Ipratropium Bromide by Using Rp-HPLC

Bansode¹,

Patil²,

Gaikwad³

et al. 2020

IND. DRU.

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A simple stability indicating RP-HPLC method was validated for determination of ipratropium bromide in the bulk drug. The drug was resolved using HPLC Column (Kromasil ODS 150 x 4.6 mm C18 column) with mobile phase of HPLC grade acetonitrile:potassium di-hydrogen phosphate buffer (60:40 V/V) at a flow rate of 1 ml/min. The retention time of ipratropium bromide was 3.7 min with UV detection at 254 nm. The method was validated with respect to linearity, sensitivity, accuracy, precision and robustness as per the International Conference on Harmonization (ICH) guidelines. The method was specific and it was observed that no interference with diluents. The linearity was established over the concentration range of 20-120 μg/ml with correlation coefficients (r2) 0.9958 for ipratropium bromide. The mean recovery was found to be in the range of 99.8% for ipratropium bromide. The % R.S.D. values for intraday precision study and inter-day study were <1.0%, confirming that the method was sufficiently precise. The drug was subjected to forced degradation under different conditions. The drug was degraded more in oxidative condition (28.89%) then alkaline condition (26.39%) then acidic condition (13.42%). There was no degradation seen under the thermal conditions.

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Quantitative analysis of a quaternary ammonium drug: ipratropium bromide by LC/ESI‐MSⁿ in horse plasma and urine

Cited by 3 publications

References 10 publications

LC‐HRMS/MS study of the prodrug ciclesonide and its active metabolite desisobutyryl‐ciclesonide in plasma after an inhalative administration to horses for doping control purposes

LC‐HRMS/MS study of the prodrug ciclesonide and its active metabolite desisobutyryl‐ciclesonide in plasma after an inhalative administration to horses for doping control purposes

Enrichment and analysis of quaternary alkaloids from Zanthoxylum simulans using weak cation exchange solid‐phase extraction coupled with LC–MS

Development and Validation of Stability Indicating Method for Ipratropium Bromide by Using Rp-HPLC

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Quantitative analysis of a quaternary ammonium drug: ipratropium bromide by LC/ESI‐MSn in horse plasma and urine

Cited by 3 publications

References 10 publications

LC‐HRMS/MS study of the prodrug ciclesonide and its active metabolite desisobutyryl‐ciclesonide in plasma after an inhalative administration to horses for doping control purposes

LC‐HRMS/MS study of the prodrug ciclesonide and its active metabolite desisobutyryl‐ciclesonide in plasma after an inhalative administration to horses for doping control purposes

Enrichment and analysis of quaternary alkaloids from Zanthoxylum simulans using weak cation exchange solid‐phase extraction coupled with LC–MS

Development and Validation of Stability Indicating Method for Ipratropium Bromide by Using Rp-HPLC

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Quantitative analysis of a quaternary ammonium drug: ipratropium bromide by LC/ESI‐MSⁿ in horse plasma and urine