A sensitive and precise method for determination of berberine hydrochloride (BEH) and palmatine (PAL) in human plasma and in urine simultaneously was developed using capillary electrophoresis (CE) combined with polypropylene hollow fiber liquid–liquid–liquid microextraction (PHF-LLLME). Because of the reports of human poisoning as a consequence of unregulated use of some drugs containing alkaloids, development of a rapid and precise assay for alkaloid measurement in the clinical setting is desirable. We report herein the development of a sensitive and precise assay for the measurement of alkaloids in the setting of a clinic. Ten participants (6 men and 4 women with a mean age of 26.3) who resided in a closed research unit participated in the detection of alkaloids. All of the volunteers were healthy. BEH and PAL were selected as model compounds to develop and evaluate the performance of the proposed method. Under the optimum conditions, the linear range was 20–1600 ng mL−1 for BEH, and 50–1600 ng mL−1 for PAL. The limits of quantification for BEH and PAL were found to be 8.7 and 11.3 ng mL−1, respectively. The average extraction recoveries in urine ranged from 87.3 to 102.4% and in plasma ranged from 78.2 to 109.7%. The RSDs were less than 4.2 and 10.5, respectively. The proposed method greatly improves the extraction efficiency and simplifies the experimental procedure considerably, and can be used as an automatic process for quantitative determination of alkaloids in a clinical setting.
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