Validation and application of a quantitative liquid chromatography tandem mass spectrometry assay for the analysis of rifapentine and 25-O-desacetyl rifapentine in human milk

Mkhize, Buyisile; Kellermann, Tracy; Norman, Jennifer; Castel, Sandra; Joubert, Anton; Merwe, Marthinus van der; Dooley, Kelly E.; Mathad, Jyoti S.; Wiesner, Lubbe

doi:10.1016/j.jpba.2022.114774

Cited by 5 publications

(2 citation statements)

References 19 publications

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“…11–14 However, previously reported methods for the detection of rifamycin antibiotics and their active metabolites require complex sample preparation procedures and long analytical times. 15,16…”

Section: Introductionmentioning

confidence: 99%

“…[11][12][13][14] However, previously reported methods for the detection of rifamycin antibiotics and their active metabolites require complex sample preparation procedures and long analytical times. 15,16 Herein, we present a rapid, sensitive, and simple ultrahigh-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS)-based method for simultaneous analysis of RFP, RBT, RFPT, and their active metabolites in human plasma using a gradient program with uncomplicated mobile phases and 1-step protein precipitation with acetonitrile. The developed method involves a convenient pretreatment step and requires short analytical time.…”

Section: Introductionmentioning

confidence: 99%

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Simultaneous Determination of Rifamycin Antibiotics and Their Active Metabolites in Human Plasma Using UHPLC-MS/MS to Evaluate Their Impact on Target Peak Concentrations: A Short Communication

Zhang

et al. 2023

Therapeutic Drug Monitoring

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Background: Standard and proper antituberculosis (anti-TB) treatment is essential for patients with TB, and rifamycin antibiotics are key components of anti-TB therapy. Therapeutic drug monitoring (TDM) of rifamycin antibiotics can shorten the time to response and complete treatment of TB. Notably, antimicrobial activities of the major active metabolites of rifamycin are similar to those of their parent compounds. Thus, a rapid and simple assay was developed for simultaneous determination of rifamycin antibiotics and their major active metabolites in plasma to evaluate their impact on target peak concentrations. Here, the authors have developed and validated a method for simultaneous determination of rifamycin antibiotics and their active metabolites in human plasma using ultrahighperformance liquid chromatography tandem mass spectrometry.Methods: Analytical validation of the assay was performed in accordance with the bioanalytical method validation guidance for industry described by the US Food and Drug Administration and the guidelines for bioanalytical method validation described by the European Medicines Agency. Results:The drug concentration quantification method for rifamycin antibiotics, including rifampicin, rifabutin, and rifapentine, and their major active metabolites was validated. Significant differences in the proportions of active metabolites in rifamycin antibiotics may affect the redefinition of their effective concentration ranges in the plasma. The method developed herein is expected to redefine the ranges of "true" effective concentrations of rifamycin antibiotics (including parent compounds and their active metabolites). Conclusions:The validated method can be successfully applied for high-throughput analysis of rifamycin antibiotics and their active metabolites for TDM in patients receiving anti-TB treatment regimens containing these antibiotics. Proportions of active metabolites in rifamycin antibiotics markedly varied among individuals. Depending on the clinical indications of patients, the therapeutic ranges for rifamycin antibiotics may be redefined.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Simultaneous Determination of Rifamycin Antibiotics and Their Active Metabolites in Human Plasma Using UHPLC-MS/MS to Evaluate Their Impact on Target Peak Concentrations: A Short Communication

Zhang

et al. 2023

Therapeutic Drug Monitoring

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Application of a kosmotrope (Na₂CO₃) and chaotrope (NaCl) in chemometric optimization of aqueous two‐phase extraction of bioactive compounds in Hypoxis iridifolia

Lukheli,

Tavengwa,

Mokgehle

2024

Analytical Science Advances

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Enterolactone, coumaric acid and vitexin are polyphenolic compounds present in a variety of fruits, vegetables, cereals and plants. These bioactive compounds are in high demand due to their antioxidant property in various tissues and organs. The purpose of this study was to develop a simultaneous extraction method, an aqueous two‐phase extraction (ATPE) method, that would enable the extraction of these compounds from Hypoxis iridifolia. This environmentally friendly extraction method only applied water and ethanol as extraction solvents for these analytes from the plant matrix. After phase separation, the analytes were salted‐out from the aqueous phase into the organic phase with the aid of a chaotrope (NaCl) or kosmotrope (Na2CO3). Thereafter, the analytes were withdrawn by a micro‐pipette for analysis on the high‐performance liquid chromatography–photodiode array detector. Optimization was conducted using a central composite design, where three parameters were examined which involved percentage ethanol, centrifugation time and salt type. Generally, the optimized conditions for extraction were an ethanol percentage of 100% and a centrifugation time of 10 min, which yielded concentrations of 2942, 23,823 and 8881 mg kg−1 for enterolactone, vitexin and coumaric acid, respectively, in the presence of a kosmotrope. The optimized conditions of extraction in the presence of chaotrope were an ethanol percentage of 66% and a centrifugation time of 10 min with concentrations of 6727, 20,833 and 8618 mg kg−1 for enterolactone, vitexin and coumaric acid, respectively. The ATPE method involving Na2CO3 was a better extractant of all the compounds studied relative to that of NaCl. The superior extraction capability of Na2CO3 in ATPE could serve as a prototype for the development of efficient extraction methods to meet the high demand for medicinal compounds derived from natural products.

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Characterization and chemometric based optimization of bioactive metabolites in Hypoxis hemerocallidea with the aid of UPLC-QqQ-MS/MS

Shikweni,

Tavengwa,

Mokgehle

2023

Chem. Pap.

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Abstractβ-sitosterol and solasodine are major bioactive ingredients in Hypoxis hemerocallidea (H. hemerocallidea) with significant pharmacological properties. As a result, developing a simple and efficient extraction method for simultaneous extraction of both analytes is critical. The purpose of this study was to identify and separate β-sitosterol and solasodine from ethanolic extracts of H. hemerocallidea using a modified QuEChERS method and subsequent analysis via UPLC triple quadrupole mass spectrometry. Response surface methodology was carried out, which included numerical parameters such as ultrasonication time, centrifugation time, and ultrasonication power. The categorical factors included the type of salt used to facilitate extraction, which was (NH4)2SO4 and Na2SO4. Fitting the response surface model to the experimental data produced a quadratic model with a good fit (R2 = 0.9966 for solasodine and R2 = 0.9857 for β-sitosterol). The optimum conditions for extraction of β-sitosterol and solasodine were an ultrasonication time of 30 min, ultrasonication power of 300 W and centrifugation time of 12 min. The generally higher concentrations of analytes obtained for (NH4)2SO4 indicated that it had a superior salting-out ability compared to Na2SO4. In conclusion, for the first time, β-sitosterol and solasodine were simultaneously extracted using modified QuEChERS with good yields through the salting-out action of (NH4)2SO4 in the presence of environmentally friendly solvents, ethanol and water. This modified QuEChERS technique can potentially be applied on a large scale as a sustainable and quick method for enrichment of therapeutic compounds from natural products.

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Validation and application of a quantitative liquid chromatography tandem mass spectrometry assay for the analysis of rifapentine and 25-O-desacetyl rifapentine in human milk

Cited by 5 publications

References 19 publications

Simultaneous Determination of Rifamycin Antibiotics and Their Active Metabolites in Human Plasma Using UHPLC-MS/MS to Evaluate Their Impact on Target Peak Concentrations: A Short Communication

Simultaneous Determination of Rifamycin Antibiotics and Their Active Metabolites in Human Plasma Using UHPLC-MS/MS to Evaluate Their Impact on Target Peak Concentrations: A Short Communication

Application of a kosmotrope (Na₂CO₃) and chaotrope (NaCl) in chemometric optimization of aqueous two‐phase extraction of bioactive compounds in Hypoxis iridifolia

Characterization and chemometric based optimization of bioactive metabolites in Hypoxis hemerocallidea with the aid of UPLC-QqQ-MS/MS

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Validation and application of a quantitative liquid chromatography tandem mass spectrometry assay for the analysis of rifapentine and 25-O-desacetyl rifapentine in human milk

Cited by 5 publications

References 19 publications

Simultaneous Determination of Rifamycin Antibiotics and Their Active Metabolites in Human Plasma Using UHPLC-MS/MS to Evaluate Their Impact on Target Peak Concentrations: A Short Communication

Simultaneous Determination of Rifamycin Antibiotics and Their Active Metabolites in Human Plasma Using UHPLC-MS/MS to Evaluate Their Impact on Target Peak Concentrations: A Short Communication

Application of a kosmotrope (Na2CO3) and chaotrope (NaCl) in chemometric optimization of aqueous two‐phase extraction of bioactive compounds in Hypoxis iridifolia

Characterization and chemometric based optimization of bioactive metabolites in Hypoxis hemerocallidea with the aid of UPLC-QqQ-MS/MS

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Application of a kosmotrope (Na₂CO₃) and chaotrope (NaCl) in chemometric optimization of aqueous two‐phase extraction of bioactive compounds in Hypoxis iridifolia