士的宁及马钱子碱清洁残留物的中空纤维液相微萃取-高效液相色谱法测定

Determination of Strychnine and Brucine in Cleaning Residue by Hollow Fiber-Liquid Phase Microextraction and HPLC

马钱子常见于中药制剂，其主要活性成分为士的宁（1）和马钱子碱（2），均为叔胺结构，难溶于水，具有强毒性，其有效剂量和中毒剂量非常接近，易发生中毒。因此必须对这些中药制剂的生产设备进行严格的清洗，并且还要对其生产废水中的痕量1和2预处理，合格后才能排放。

A hollow fiber-liquid phase microextraction （HF-LPME）-HPLC method was established for the determination of trace strychnine and brucine in cleaning validation of productional equipment. Parameters influencing the extraction efficiency were investigated and optimized. The enrichment factors of strychnine and brucine were 80.6 and 122.4, respectively, under extraction by n-octyl alcohol and agitating at 800 r/min for 60 min. An HPLC method was applied for the determination. A C^8 column was used with the mobile phase of 0.4% phosphoric acid （adjusted to pH 3.0 by triethylamine）-acetonitrile （85 ： 15） at the detection wavelength of 260 nm. The calibration curves for strychnine and brucine were linear in the range of 0.01 - 1μg/ml. Their recoveries were 98.3 % and 98.5 %, with RSDs of 0.4 % and 0.6%.