LC-QQQ/MS结合色差技术优选炒蒺藜饮片的炮制工艺  

Optimization of Processing Technology for Stir-fried Tribuli Fructus Pieces by LC-QQQ/MS Combined with Chromatic Aberration Technology

作　　者：孙晓晨 王丽丽 王书月 王帅 刘坤琳 张超[1] SUN Xiaochen;WANG Lili;WANG Shuyue;WANG Shuai;LIU Kunlin;ZHANG Chao(College of Pharmacy,Shandong University of Traditional Chinese Medicine,Jinan 250355,China;Shandong Hongjitang Pharmaceutical Group Co.,Ltd.,Jinan 250103,China)

机构地区：[1]山东中医药大学药学院,济南250355 [2]山东宏济堂制药集团股份有限公司,济南250103

出　　处：《中国现代应用药学》2022年第16期2063-2068,共6页Chinese Journal of Modern Applied Pharmacy

基　　金：国家自然科学基金青年科学基金项目(81603298);国家中医药管理局全国中医药创新骨干人才培训项目(国中医药人教函[2019]128号);山东省中医药科技发展计划项目(2019-0028);山东省重点研发计划项目(2019GSF108171)。

摘　　要：目的建立一种蒺藜甾体皂苷含量测定和外观颜色均匀性检测方法来优化炒蒺藜炮制工艺。方法以LC-QQQ/MS测定蒺藜呋甾皂苷B和蒺藜皂苷K的总含量作为化学指标,采用色彩色差仪测定炒蒺藜饮片总色值Ε*ab,以30次随机抽取样品Ε*ab值的RSD值作为外观颜色均匀性指标。在此基础上,采用L9(3~4)正交试验法,以炒制温度、炒制时间和炒药机转速为考察因素,优选炒蒺藜饮片的炮制工艺。结果蒺藜呋甾皂苷B和蒺藜皂苷K均具有良好的线性关系(r>0.999),检测限分别为1.28,10.44 ng·mL^(-1),定量限分别为5.40,27.81 ng·mL^(-1),精密度、24 h稳定性、重复性试验的RSD均<3.0%,平均加样回收率分别为96.66%和97.10%。色差技术可为炒蒺藜外观颜色均匀性提供客观化的数值。炒蒺藜最佳炮制工艺为200℃以60 r·min^(-1)转速炒制15 min。结论LC-QQQ/MS结合色差技术所优选的蒺藜炒制工艺稳定可行,可为其他中药炮制工艺优化提供参考。OBJECTIVE To establish a method for determining the content of steroidal saponins of Tribuli Fructus and the uniformity of appearance color to optimize the processing technology of stir-fried Tribuli Fructus.METHODS Using LC-QQQ/MS method to determine the total content of terrestroside B and terrestrosin K as chemical indicators.Using colorimeter determination to determine the Ε* ab value of stir-fried Tribuli Fructus,and the 30 random samples’ RSDs of the Ε* ab value were taken as the indicator of the appearance color uniformity.On this basis,the processing technology of stir-fried Tribuli Fructus was optimized by L9(3~4) orthogonal test with the frying temperature,frying time and speed of the frying machine as the inspection factors.RESULTS Both of terrestroside B and terrestrosin K showed good linear relationships(r>0.999).LODs were 1.28 ng·mL^(-1) and 10.44 ng·mL^(-1),LOQs were 5.40 ng·mL^(-1) and 27.81 ng·mL^(-1).Precision,stability in 24 h and reproducibility of this method were satisfactory and RSDs were all < 3.0%.The average recoveries were 96.66% and 97.10%,respectively.Chromatic aberration technology could provide objective value for the appearance color uniformity of stir-fried Tribuli Fructus.The optimum processing technology of stir-fried Tribuli Fructus was stir-fried at 60 r·min^(–1) at 200 ℃ for 15 min.CONCLUSION The optimized processing technology of stir-fried Tribuli Fructus by LC-QQQ/MS combined with chromatic aberration technology is stable and feasible,which can provide reference for the optimization of processing technology of other Chinese medicine.

关 键 词：蒺藜 LC-QQQ/MS 色差技术 炒制工艺 蒺藜呋甾皂苷B 蒺藜皂苷K 

分 类 号：R283.3[医药卫生—中药学]