Proposed Selection Strategy of Surrogate Matrix to Quantify Endogenous Substances by Japan Bioanalysis Forum DG2015-15

Wakamatsu, Akira; Ochiai, Shoko; Suzuki, Eiko; Yokota, Yoshinobu; Ochiai, Midori; Kotani, Yosuke; Sasahara, Satomi; Nakanaga, Keita; Hashimoto, Yuki; Ueno, Satoko; Kato, Nozomu; Kawada, Satoshi; Hayakawa, Jun-ichiro; Shimada, Eiichi; Horita, Shinya; Sakai, Kazuaki

doi:10.4155/bio-2018-0105

Cited by 29 publications

(15 citation statements)

References 2 publications

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“…Calibration curves also need particular attention and it is always preferred to prepare them in the correspondent matrix of analysis due to the possible matrix effects caused by co-eluting matrix components. An analytical problem arises when the quantification involves endogenous compounds where it is important to select an appropriate surrogate matrix which is a matrix whose composition is identical to the analyzed samples but with the absence of the analyte [38]. Although caffeine and its metabolites are exogenous compounds, the same challenge of obtaining human plasma without the compounds of interest occurs during the method validation process.…”

Section: Introductionmentioning

confidence: 99%

Validation of an LC-MS/MS Method for the Quantification of Caffeine and Theobromine Using Non-Matched Matrix Calibration Curve

et al. 2019

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Caffeine is one of the most widely consumed psycho-stimulants. The study of the beneficial effects of caffeine consumption to decrease the risk of developing several neuropsychiatric pathologies is receiving increasing attention. Thus, accurate and sensitive methods have been developed, mainly by LC-MS/MS, in order to quantify caffeine and its metabolites. These quantifications of caffeine and its metabolites by LC-MS/MS require a considerable effort to select or find a surrogate matrix, without the compounds of interest, to be used in the calibration curves. Thus, we evaluated the possibility of using calibration curves prepared in solvent instead of calibration curves prepared in human plasma. Results show that the calibration curves prepared in solvent and in human plasma were similar by comparing their slopes and interceptions, and the accuracy and precision were within the limits of acceptance for both calibration curves. This work demonstrates that, by using internal standards, it is possible to use a calibration curve in solvent instead of a calibration curve in plasma to perform an accurate and precise quantification of caffeine and theobromine.

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Section: Introductionmentioning

confidence: 99%

Validation of an LC-MS/MS Method for the Quantification of Caffeine and Theobromine Using Non-Matched Matrix Calibration Curve

et al. 2019

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“…Thus, with this study, the sensitive, comprehensive and simultaneous determination of all active kinin peptides with their major metabolites is facilitated for the first time in plasma. An ideal surrogate matrix should closely resemble the study samples and be analyte-free [32]. Previous LC-MS/ MS assays for bradykinin used water [19] or bovine plasma as a surrogate matrix due to the endogenous presence of kinins in human matrix [21].…”

Section: Discussionmentioning

confidence: 99%

“…Previous LC-MS/ MS assays for bradykinin used water [19] or bovine plasma as a surrogate matrix due to the endogenous presence of kinins in human matrix [21]. However, different compositions of a surrogate matrix in comparison to study samples might lead to matrix effects affecting the accuracy of the results [32]. Therefore, a better approach is provided by the use of standard addition for bradykinin, as reported by Lame et al 2016 [20].…”

Section: Discussionmentioning

confidence: 99%

Targeted LC-MS/MS platform for the comprehensive determination of peptides in the kallikrein-kinin system

Gangnus

Burckhardt

2021

Anal Bioanal Chem

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The kallikrein-kinin system (KKS) is involved in many physiological and pathophysiological processes and is assumed to be connected to the development of clinical symptoms of angioedema or COVID-19, among other diseases. However, despite its diverse role in the regulation of physiological and pathophysiological functions, knowledge about the KKS in vivo remains limited. The short half-lives of kinins, their low abundance and structural similarities and the artificial generation of the kinin bradykinin greatly hinder reliable and accurate determination of kinin levels in plasma. To address these issues, a sensitive LC-MS/MS platform for the comprehensive and simultaneous determination of the four active kinins bradykinin, kallidin, des-Arg(9)-bradykinin and des-Arg(10)-kallidin and their major metabolites bradykinin 2-9, bradykinin 1-7 and bradykinin 1-5 was developed. This platform was validated according to the bioanalytical guideline of the US Food and Drug Administration regarding linearity, accuracy, precision, sensitivity, carry-over, recovery, parallelism, matrix effects and stability in plasma of healthy volunteers. The validated platform encompassed a broad calibration curve range from 2.0–15.3 pg/mL (depending on the kinin) up to 1000 pg/mL, covering the expected concentrations in disease states. No source-dependent matrix effects were identified, and suitable stability of the analytes in plasma was observed. The applicability of the developed platform was proven by the determination of endogenous levels in healthy volunteers, whose plasma kinin levels were successfully detected in the low pg/mL range. The established platform facilitates the investigation of kinin-mediated diseases (e.g. angioedema, COVID-19) and enables the assessment of the impact of altered enzyme activities on the formation or degradation of kinins. Graphical abstract

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“…Two qualification ion transitions were established, and the peak area ratios between the qualified and quantified ion transitions of SL were calculated. The ratios of peak area between the HQC sample in the surrogate matrix and the authentic liver and kidney tissue samples were compared and evaluated for equivalence, as described previously [25]. The 3 -SL and 6 -SL isomers were identified by comparing the retention time and ion pair transition between the standard and samples.…”

Section: Selectivitymentioning

confidence: 99%

“…LLOQ and LQC samples were prepared using a surrogate matrix. For the MQC and HQC samples, the background concentration of SL was determined by analyzing the homogenized blank minipig tissue sample, and the background concentration was subtracted from the measured concentrations [25]. The accuracies of the MQC and HQC were calculated by the following equation:…”

Section: Accuracy and Precisionmentioning

confidence: 99%

Development and Validation of a Bioanalytical Method for 3′- and 6′-Sialyllactose in Minipig Liver and Kidney Using Liquid Chromatography-Tandem Mass Spectrometry and Its Application to Analysis of Tissue Distribution

2020

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Breast milk contains human milk oligosaccharides (HMOs), including sialyllactose (SL). SL is composed of sialic acid and lactose, and is divided into 3′-SL and 6′-SL according to the binding position. SL has immunoprotective effects against bacteria and viruses, and acts as a probiotic in the gastrointestinal tract. In this study, we developed a bioanalytical method for simultaneous analysis of 3′-SL and 6′-SL in liver and kidney tissues of Yucatan minipigs using liquid chromatography–tandem mass spectrometry (LC-MS/MS) under conditions optimized in our previous study. LC-MS/MS was performed using a hydrophilic interaction liquid chromatography (HILIC) column (50 mm × 2.1 mm, 3 μm) with a mobile phase consisting of 10 mM ammonium acetate in water (pH 4.5) and acetonitrile with gradient elution at a flow rate of 0.3 mL/min. A surrogate matrix method using water was applied for analysis of endogenous SL. The developed method was validated with regard to selectivity, linearity, precision, accuracy, the matrix effect, recovery, parallelism, dilution integrity, carryover, and stability according to the US Food and Drug Administration guidelines. We performed a tissue distribution study of minipigs, and analyzed liver and kidney tissues using the developed method to determine the tissue distribution of 3′-SL and 6′-SL. The tissue concentrations of 3′-SL and 6′-SL were readily measurable, suggesting that the method would be useful for evaluating the tissue distributions of these compounds in minipigs.

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Proposed Selection Strategy of Surrogate Matrix to Quantify Endogenous Substances by Japan Bioanalysis Forum DG2015-15

Cited by 29 publications

References 2 publications

Validation of an LC-MS/MS Method for the Quantification of Caffeine and Theobromine Using Non-Matched Matrix Calibration Curve

Validation of an LC-MS/MS Method for the Quantification of Caffeine and Theobromine Using Non-Matched Matrix Calibration Curve

Targeted LC-MS/MS platform for the comprehensive determination of peptides in the kallikrein-kinin system

Development and Validation of a Bioanalytical Method for 3′- and 6′-Sialyllactose in Minipig Liver and Kidney Using Liquid Chromatography-Tandem Mass Spectrometry and Its Application to Analysis of Tissue Distribution

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