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目的:建立HPLC法并对二十五味鬼臼丸中的鬼臼毒素进行含量测定。方法:采用Shim-pack VP-ODS C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.2%磷酸水溶液为流动相,线性梯度洗脱(0~10 min,35%乙腈;10~25 min,35%乙腈→55%乙腈;25~30 min,55%乙腈→35%乙腈),流速1.0 m L·min~(-1),检测波长290 nm,柱温30℃。结果:鬼臼毒素的线性范围为0.02~0.33μg(r=0.999 9),方法回收率(n=6)为100.5%(RSD=0.57%)。全国7个生产企业的69批次二十五味鬼臼丸中鬼臼毒素含量范围为0.02~0.77 mg·g~(-1);二十五味鬼臼丸中鬼臼毒素含量限度定为0.07 mg·g-1。结论:本方法制定了二十五味鬼臼丸处方中主药鬼臼中鬼臼毒素的含量限度,为该药的质量控制提供了有力的依据。
Objective: To establish an HPLC method and to determine the content of podophyllotoxin in Twenty-five flavor tablets. METHODS: A linear gradient elution was carried out on a Shim-pack VP-ODS C18 column (250 mm × 4.6 mm, 5 μm) using a mobile phase of acetonitrile-0.2% phosphoric acid (0-10 min, 35% min, 35% acetonitrile → 55% acetonitrile; 25-30 min, 55% acetonitrile → 35% acetonitrile) at a flow rate of 1.0 mL · min -1. Results: The linear range of podophyllotoxin was 0.02-0.33 μg (r = 0.999 9). The recovery rate was 100.5% (RSD = 0.57%). The content of podophyllotoxin in 69 batches of Twenty Wuwei Weiwu pills treated by 7 manufacturing enterprises in China was 0.02-0.77 mg · g -1. The content of podophyllotoxin in Twenty Wuwei Weiju pills was defined as 0.07 mg · g-1. CONCLUSION: The method has established the limit of podophyllotoxin in the main drug podophyllotoxin in Twenty-five-flavored Potion pill prescription, which provides a strong basis for the quality control of this drug.