高效液相色谱法测定川贝母和川贝粉中三嗪代谢物残留

Determination of triazine metabolites in Fritillaria chuanensis and tendrilleaf fritillary shell powder by high performance liquid chromatography

中文关键词:  三嗪代谢物  高效液相色谱  中药材  川贝

英文关键词:triazine metabolite  high performance liquid chromatography  Chinese medicinal materials  fritillaria chuanensis

中文摘要:

      目的 建立了一种快速固相萃取联合高效液相色谱法同时测定川贝母和川贝粉中3种三嗪代谢物残留量的分析方法。方法 采用分散固相萃取前处理方法, 样品经乙腈-水提取, 无水硫酸镁和醋酸钠等无机盐盐析分离, 十八烷基硅烷键合硅胶C18净化处理, 以Athena C18柱为色谱柱, 以水和乙腈为流动相进行梯度洗脱, 外标法定量。结果 通过合理选择色谱柱、流动相和净化剂, 在最佳色谱条件下, 脱异丙基莠去津、脱乙基莠去津和脱乙基特丁津等3种三嗪代谢物的检出限为0.20 μg/kg, 定量限为0.67 μg/kg, 3种目标组分在0.01~20.00 μg/mL的线性范围内线性关系良好(r≥0.999), 在5、25和50 μg/kg 3个添加水平内, 平均加标回收率为95.3%~105.7%, 相对标准偏差为1.0%~2.4%。结论 该方法简单、快速、灵敏, 适用于川贝类中药材中三嗪类农药代谢物残留量的快速检测分析。

英文摘要:

      Objective To set up a rapid solid phase extraction combined high performance liquid chromatography (HPLC) method and the measuring unibract fritillary bulb of fritillary bulb powder in three triazine metabolites residues analysis methods. Methods The samples were extracted by acetonitrile-water, separated by inorganic salts such as anhydrous magnesium sulfate and sodium acetate, purified by octyl-bonded silica gel C18 Athena C18 column was used as the chromatographic column, water and acetonitrile were used as the mobile phase for gradient elution and quantitative determination by external standard method. Results By selecting the appropriate chromatographic column, mobile phase, and purification agent, under the optimal chromatographic conditions, the metabolism of three triazine metabolites, namely isopropylatrazine, diethylatrazine, and diethylterbutazine, the limits of detection and quantitation of the 3 kinds of triazine metabolites were 0.20 μg/kg and 0.67 μg/kg respectively. The linear relationship of the three target components was good (r≥0.999) in the linear range of 0.01–20.00 μg/mL. The average recoveries were 95.3%~105.7% and relative standard deviation were 1.0%–2.4% in the addition levels of 5.0、25 and 50 μg/kg. Conclusion The method is simple, rapid and sensitive, and is suitable for the rapid detection and analysis of triazine pesticide metabolites in the traditional Chinese medicinal materials.