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Determination of ligustrazine in rat serum by polymer monolithic micro-extraction combined with ultra high performance liquid chromatography-tandem mass spectrometry

Sun Danling, Peng Xitian, Peng Maomin, Zhang Xian, Xia Hong, Xu Zhimin, Hu Xizhou

Acta Chromatographica

2021

Vol. 33, no. 3

253--260

This study focused on developing an effective and environmentally friendly method to measure ligustrazine in rat serum by using polymer monolith micro-extraction (PMME) technique. A poly (methacrylic acid-ethylene glycol dimethacrylate) material was used to extract ligustrazine through hydrophobic and ion-exchange interaction. Qualitative and quantitative analysis was performed by a liquid chromatography and tandem mass spectrometry. After optimization of several PMME conditions, the developed method exhibited excellent extraction performance to the ligustrazine. Good linearity was acquired ranging from 10 to 2,000 ng mL−1, and the limit of detection of the proposed method was 0.14 ng mL−1. The recoveries measured by spiking three different concentrations in rat serum ranged from 82.6 to 95.3%, and excellent precision was found with relative standard deviations (RSDs) less than 8.3% for intra-day and 9.7% for inter-day, respectively. At last, the applicability of the method was further confirmed through continuous monitoring of ligustrazine in rat serum after dosing of ligustrazine tablets to rats.

An improved UPLC method for determining uric acid in rat serum and comparison study with commercial colorimetric kits

Wen Shaoshi, Zhang Zixin, Chen Xiaopeng, Liu Jinchang, Yu Haiyang, Han Lifeng, Jin Lijun, Zhang Yi, Wang Tao

Acta Chromatographica

2019

Vol. 31, no. 3

201--205

Uric acid (UA) is the final product of purine metabolism in humans. Elevated serum UA levels lead to the development of hyperuricemia, gout, kidney diseases, and metabolic syndrome. Accurate determination of UA plays a critical role in clinical diagnosis and laboratory investigation. An ultra-performance liquid chromatography (UPLC) with ultraviolet detection method has been developed and validated for UA analysis. Separation was achieved by a Waters ethylene bridged hybrid (BEH) Amide column (50 mm × 2.1 mm i.d., 1.7 μm) with acetonitrile and 0.1% acetic acid in deionized water in the proportion of 90 to 10 (v/v) as the mobile phase. The limit of detection and limit of quantification were 0.09 and 0.18 μmol/L, respectively. The method was validated by evaluating recovery (98.37–104.20%), accuracy (0.47–0.90%), and precision (1.24–1.81% for intra-batch and 1.76–3.98% for inter-batch). This method was then applied to UA determination in rat serum of hyperuricemia model. The results from UPLC, high-performance liquid chromatography (HPLC), and uric acid kits (phosphor-tungstic acid-based kit and uricase-based kit) were compared. The UPLC results were in very good agreement with HPLC. The developed method could be employed as a useful tool for the determination of UA in biofluids.