Comparison of different linear calibration approaches for LC–MS bioanalysis

Tan, Aimin; Awaiye, Kayode; Jose, Besy; Joshi, P.; Trabelsi, Fethi

doi:10.1016/j.jchromb.2012.11.008

Cited by 14 publications

(10 citation statements)

References 32 publications

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“…Materials and Reagents. BMS-790052 (daclatasvir) and 13 C 2 15 N 4 -daclatasvir were synthesized at Bristol-Myers Squibb. Formic acid (SupraPur grade), methyl tert-butyl ether (MTBE), and dimethyl sulfoxide (DMSO) were purchased from EMD Chemicals (Gibbstown, NJ, USA).…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

“…Therefore, to improve the assay throughput and robustness, it is highly desired to simplify and, if possible, eliminate the steps for preparation of multisample external calibration curves and dilution of study samples. Several groups have reported their efforts to simplify the preparation of multisample external calibration curves by using one- or two-point calibration curves − and to eliminate the dilution of study samples by expending the calibration curve ranges , or using internal standard tracked dilution …”

Section: Introductionmentioning

confidence: 99%

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Eliminating Preparation of Multisample External Calibration Curves and Dilution of Study Samples Using the Multiple Isotopologue Reaction Monitoring (MIRM) Technique in Quantitative LC-MS/MS Bioanalysis

Zhao

DeMichele

et al. 2019

Anal. Chem.

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Preparation of multisample external calibration curves and dilution of study samples are critical steps in bioanalytical sample processing for quantitative liquid chromatography–tandem mass spectrometry (LC-MS/MS) based bioanalysis of small-molecule compounds, biotherapeutics, and biomarkers, but they can be time-consuming and prone to error. It is highly desired to simplify or eliminate these two steps in order to improve the assay throughput and robustness. While multisample external calibration curve preparation using authentic matrices can be eliminated with a previously reported in-sample calibration curve (ISCC) approach using multiple isotopologue reaction monitoring (MIRM) of a stable isotopically labeled (SIL) analyte, dilution of study samples is still inevitable due to limited LC-MS/MS assay ranges. In this work, a one-sample multipoint external calibration curve and isotope sample dilution, both using MIRM of an analyte, for quantitative LC-MS/MS based bioanalysis are proposed and demonstrated. By spiking a known amount of an analyte into one blank authentic matrix sample, a one-sample multipoint external calibration curve in an authentic matrix can be established on the basis of the relationship between the calculated theoretical isotopic abundances (analyte concentration equivalents) and the MS/MS responses in the corresponding MIRM channels. This one-sample multipoint external calibration curve can be used in the same way as the traditional multisample external calibration curve for quantitative LC-MS/MS-based bioanalysis. As isotopic abundance in each MIRM channel can be calculated and measured accurately, isotope sample dilution can be achieved by simply monitoring one or a few of the MIRM channels of the analyte in addition to the most abundant MIRM channel for study samples. While the most abundant MIRM channel (isotopic abundance of 100%) is used for the quantitation of samples having concentrations within the assay calibration curve range, less abundant MIRM channels (isotopic abundance of IA%) can be used for the quantitation of samples having concentrations beyond the assay upper limit of quantitation (ULOQ), resulting in isotope dilution factors (IDF) of 100%/IA%. The approaches of one-sample multipoint external calibration curve and isotope sample dilution were evaluated and demonstrated in this work with an example of the quantitation of daclatasvir in human plasma extracted with liquid–liquid extraction. Using these approaches together with the MIRM-ISCC methodology, accurate and reliable LC-MS/MS bioanalysis can be achieved without the need of preparation of multisample external calibration curve and dilution of study samples.

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Section: ■ Experimental Sectionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Eliminating Preparation of Multisample External Calibration Curves and Dilution of Study Samples Using the Multiple Isotopologue Reaction Monitoring (MIRM) Technique in Quantitative LC-MS/MS Bioanalysis

Zhao

DeMichele

et al. 2019

Anal. Chem.

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show abstract

“…were additionally used for assessing accuracy and precision in order to check whether one-point [32] or two-point [33] calibration could be applicable saving time and resources. For the calibration standards, the back-calculated concentrations fulfilled the acceptance criteria of EMA (accuracy: bias ≤ 15%, ≤ 20% at LLOQ; precision: CV ≤ 15%, ≤ 20% at LLOQ).…”

Section: Calibration Modelmentioning

confidence: 99%

“…In order to evaluate two-point calibration, accuracy and precision data for the QC samples (Table 3) were calculated using calibrator pair 1/6, chosen according to Tan et al [33]. These data were systematically compared to the respective results calculated with full linear calibration ignoring zero as described above, as this calibration was superior to that through zero.…”

Section: Accuracy and Precisionmentioning

confidence: 99%

“…Neither the t tests nor the F tests provided significant differences (p<0.05) at all concentration levels. Thus, two-point calibration (y = 0.0001042x + 0.009397) was accepted as the method of choice for routine testing saving time and resources [33]. and do not need to be stored for a long time or subjected to freeze-thaw cycles.…”

Section: Accuracy and Precisionmentioning

confidence: 99%

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Development and validation of a UHPLC–MS/MS procedure for quantification of the Pseudomonas Quinolone Signal in bacterial culture after acetylation for characterization of new quorum sensing inhibitors

Maurer

Steinbach

Hartmann

2013

Journal of Pharmaceutical and Biomedical Analysis

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The appearance of antibiotic resistance requires novel therapeutic strategies. One approach is to selectively attenuate bacterial pathogenicity by interfering with bacterial cell-to-cell communication known as quorum sensing. The PQS quorum sensing system of Pseudomonas aeruginosa employs as signal molecule the Pseudomonas Quinolone Signal (PQS; 2-heptyl-3-hydroxy-4-(1H)-quinolone), a key contributor to virulence and biofilm formation. Thus, interference with PQS production is considered as promising approach for the development of novel anti-infectives. Therefore, in this study, we developed and validated an ultra-high performance liquid chromatographic-tandem mass spectrometric approach for reliable quantification of PQS in P. aeruginosa cultures for activity determination of new quorum sensing inhibitors. The poor chromatographic properties of PQS reported by others could be overcome by fast microwave-assisted acetylation. The validation procedure including matrix effects, recovery, process efficiency, selectivity, carry-over, accuracy and precision, stability of the processed sample, and limit of quantification demonstrated that the method fulfilled all requirements of common validation guidelines. Its applicability was successfully proven in routine testing. In addition, two-point calibration was shown to be applicable for fast and reliable PQS quantification saving time and resources. In summary, the described method provides a powerful tool for the discovery of new quorum sensing inhibitors as potential anti-infectives and illustrated the usefulness of chemical derivatization, acetylation, in liquid chromatography-mass spectrometry analysis.

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Use of Internal Standards in LC‐MS Bioanalysis

Tan

Awaiye

2013

Handbook of LC‐MS Bioanalysis

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Comparison of different linear calibration approaches for LC–MS bioanalysis

Cited by 14 publications

References 32 publications

Eliminating Preparation of Multisample External Calibration Curves and Dilution of Study Samples Using the Multiple Isotopologue Reaction Monitoring (MIRM) Technique in Quantitative LC-MS/MS Bioanalysis

Eliminating Preparation of Multisample External Calibration Curves and Dilution of Study Samples Using the Multiple Isotopologue Reaction Monitoring (MIRM) Technique in Quantitative LC-MS/MS Bioanalysis

Development and validation of a UHPLC–MS/MS procedure for quantification of the Pseudomonas Quinolone Signal in bacterial culture after acetylation for characterization of new quorum sensing inhibitors

Use of Internal Standards in LC‐MS Bioanalysis

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