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

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

Key words:  Tribuli Fructus  LC-QQQ/MS  chromatic aberration technology  frying process  terrestroside B  terrestrosin K

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E^* ab,以30次随机抽取样品E^* ab值的RSD值作为外观颜色均匀性指标。在此基础上,采用L₉(3⁴)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。

Abstract:

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 E^* ab value of stir-fried Tribuli Fructus,and the 30 random samples'RSDs of the E^* 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(3⁴) 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.