A post-chemiluminescence (PCL) phenomenon was observed when palmatine was injected in a mixture of <i>N</i>-bromosuccinimide (NBS) and alkaline dichlorofluorescein (DCF) after the chemiluminescence (CL) reaction of NBS-alkaline DCF had finished. Based on the PCL reaction, a rapid and sensitive method for the determination of palmatine was established. Under optimum conditions, the CL intensity was linear, with the concentration of palmatine in the range of 5.0 × 10<sup>?9</sup> to 1.0 × 10<sup>?6</sup> M. The detection limit was 6.0 × 10<sup>?10</sup> M for palmatine. The relative standard deviation for 11 parallel measurements of 1.0 × 10<sup>?7</sup> M palmatine was 1.5%. This method was applied to the determination of palmatine in pharmaceutical samples and biological fluids, with satisfactory results. The possible reaction mechanism is discussed briefly.

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