Capillary Electrophoresis-Mass Spectrometry with Multisegment Injection and In-Capillary Preconcentration for High-Throughput and Sensitive Determination of Therapeutic Decapeptide Triptorelin in Pharmaceutical and Biological Matrices.
Piešťanský. Juraj J; Čižmárová. Ivana I; Štefánik. Ondrej O; Matušková. Michaela M; Horniaková. Andrea A; Majerová. Petra P; Mikuš. Peter P
Key Findings
- A new CE‑MS method with multisegment injection and field‑enhanced sample stacking was developed
- Detection limits improved 50‑fold (5 ng/mL in water, 25 ng/mL in plasma) and throughput tripled
- The method showed good linearity (R²≥0.99), precision (RSD 1.5‑11.9%) and accuracy (80‑109% recovery)
Practical Outcomes
- The test lets labs reliably track triptorelin levels for quality control or pharmacokinetic studies, but it requires specialized equipment and expertise, so it isn’t a DIY protocol for most biohackers.
Summary
Researchers created a fast, sensitive lab test that can accurately measure the peptide drug triptorelin in medicines and blood samples, using a special capillary electrophoresis‑mass spectrometry technique.
Abstract
A capillary electrophoresis-tandem mass spectrometry method with a multisegment injection and an in-capillary field-enhanced sample stacking for determination of therapeutic peptide triptorelin in pharmaceutical and biological matrices was developed. The CE separation conditions were optimized in order to obtain maximal separation efficiency, analytical signal intensity and stability, and minimal adsorption of the analyzed peptide onto the capillary wall (1 M formic acid-HFo, pH 1.88). The implementation of the field-enhanced sample injection into CE improved the value of limit of detection 50 times while the multisegment injection increased the sample throughput three times in comparison to a conventional CE approach. The proposed method was characterized by favorable performance parameters, such as linearity (r<sup>2</sup> ≥ 0.99), limit of detection (5 ng mL<sup>-1</sup> in water matrix, 25 ng mL<sup>-1</sup> in plasma matrix), precision (relative standard deviation, 1.5-9.4% for intraday and 2.3-11.9% for interday reproducibility), or accuracy (relative errors in the range of 80-109%). The FDA-validated method was successfully applied to the analysis of triptorelin in the commercial drug Diphereline<sup>®</sup> 0.1 mg (powder for injection) and in spiked human plasma samples. Favorable performance parameters along with proven application potentialities indicate the usefulness of the proposed method for its routine use in drug quality control laboratories and for clinical analysis, such as determination of triptorelin levels in plasma (for pharmacokinetic study).
Study Information
pubmed
2021
2021-10-16T00:00:00.000Z
10.3390/biomedicines9101488
13
53