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. 2023 Jan 9;28(2):671.
doi: 10.3390/molecules28020671.

QuEChERS-Based Approach to the Extraction of Five Calcium Channel Blockers from Plasma Determined by UPLC-MS/MS

Tingting Zhao  1 , Wen Jiang  2 , Xiaolan Zhen  3 , Chengcheng Jin  2 , Yifan Zhang  1 , Hui Li  1   3
Affiliations

QuEChERS-Based Approach to the Extraction of Five Calcium Channel Blockers from Plasma Determined by UPLC-MS/MS

Tingting Zhao et al. Molecules. .

Abstract

Here, a QuEChERS (quick, easy, cheap, effective, rugged, and safe) pretreatment method was combined with UPLC-MS/MS to facilitate the rapid and reliable simultaneous detection of five calcium channel blockers (CCBs) in human plasma. For this approach, samples were treated with 1 mL of acetonitrile, 350 mg of magnesium sulfate, and 70 mg of PSA adsorbent prior to centrifugation. Supernatants then underwent gradient elution for 8 min with an Agilent C18 column using an acetonitrile-water solution supplemented with 5 mmol⋅L-1 of ammonium acetate. This technique exhibited a good linear response in the 1-800 ng⋅mL-1 range for the analyzed drugs, with an R2≥ 0.9921, an accuracy of 87.54-113.05%, a matrix effect (ME) of 91.21-116.39%, a precision of 0.19-11.64%, and stability of no more than 10.05%. This time-saving QuEChERS reagent-based pretreatment technique thus allowed for the simultaneous and accurate detection of five CCBs in human plasma samples, providing a promising new basis for therapeutic drug monitoring in patients with hypertension.

Keywords: QuEChERS; UPLC-MS/MS; calcium channel blockers; human plasma; hypertension.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
Typical chromatograms of IS-propranolol (A), nifedipine (B), nitrendipine (C), felodipine (D), amlodipine (E), and nimodipine (F) in blank plasma samples, the chromatogram of sixblank plasma samples (G–N) and chromatogram of six blank samples after HQC sample analysis (M–R).
Figure 1
Figure 1
Typical chromatograms of IS-propranolol (A), nifedipine (B), nitrendipine (C), felodipine (D), amlodipine (E), and nimodipine (F) in blank plasma samples, the chromatogram of sixblank plasma samples (G–N) and chromatogram of six blank samples after HQC sample analysis (M–R).
Figure 2
Figure 2
(A) The area results of five CCBs treated with different extraction solvents. (B) The area results of five CCBs treated with different volumes of extractants.
Figure 3
Figure 3
(A) The area results of five CCBs treated with different purifying agents. (B) The area results of five CCBs treated with different amounts of purifying agents.
Figure 4
Figure 4
The area results of five CCBs treated with different amounts of MgSO4.
Figure 5
Figure 5
Product ion mass spectra of amlodipine (A), felodipine (B), nifedipine (C), nimodipine (D), nitrendipine (E) and IS-propranolol (F) in positive mode.
Figure 6
Figure 6
The chemical structure and possible fragmentation pathways of five CCBs.
See this image and copyright information in PMC

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