Study On The Improvement Of Quality Standard Of Compound Zhulingjianpi Capsules

ZhulingJianpi Capsule is a kind of Chinese patent medicine which is made from Drynariae Rhizoma,Phellodendri Chinensis Cortex,Paeoniae Radix Alba,Atractylodis Macrocephalae Rhizoma,Solidaginis Herba,Linderae Radix,Codonopsis Radix,Acalypha australis,Magnoliae Officinalis Cortex,Pori a,Alismatis Rhizoma,Saposhnikoviae Radix,Coicis Semen,Rhei Radix et Rhizoma,Cinnamomi Ramulus,Citri Reticulatae Pericarpium,Arecae Semen and Glycyrrhizae Radix et Rhizoma.It has the functions of invigorating spleen and tonifying kidney,regulating qi,moistening and clearing heat,and used for the treatment of diarrhea-type irritable bowel syndrome.Having a good effect on spleen and kidney qi deficiency and abdominal pain,diarrhea,fatigue,weak waist and knees,anus burning,mouth bitterness,emotional upset,etc.The current standard of Zhulingjianpi Capsule was recorded by China Food and Drug Administration.The main contents include the thin layer chromatographic identifications of six Chinese herbals:Atractylodis Macroce-phalae Rhizoma,Paeoniae Radix Alba,Rhei Radix et Rhizoma,Phellodendri Chinensis Cortex,Citri Reticulatae Pericarpium and Magnoliae Officinalis Cortex.However,there are some problems in the current standards about thin layer chromatographic identification methods of some drugs and the assay method,such as complicated operation and poor reproducibility.In order to better control the quality of Zhulingjianpi Capsule,this research has been done to optimize those methods,furthermore three new TLC identification methods separately for 3 medicinal materials,and a high-performance liquid chromatographic fingerprinting method were established.1.Establishment of TLC identification methods for seven kinds of herbs In this experiment,the test solutions for the thin layer chromatographic identification of seven kinds of herbs were prepared by a one-time extraction scheme,and the TLC methods were established accordingly.Firstly,4 g powder of Capsule contents was sonicated with n-hexane for 15 minutes,filter,and the filtrate was used as a sample solution to identify Atractylodis Macrocephalae Rhizoma;the residue was sonicated with 20 ml of methanol,filter,and 4 ml of the filtrate was evaporated to dryness and dissolve to 1 ml to identify Paeoniae Radix Alba,Phellodendri Chinensis Cortex and Citri Reticulatae Pericarpium;The rest of filtrate was evaporated to dryness,dissolved with water and transferred into a macroporous resin column with an inner diameter of 2 cm and 15 cm in length.Eluted the column with 10%methanol,and the eluent was discarded,then eluted with 50%methanol and concentrated to 1 ml,which was used to identify Linderae Radix and Saposhnikoviae Radix.Then sequentially eluted the column with 80%methanol and the eluate was concentrated to 1 ml,which was used to identify Glycyrrhizae Radix et Rhizoma;Finally eluted the column with 90%methanol and concentrated the eluent to 1 ml,which was used to identify Magnoliae Officinalis Cortex.The established method is simple in operation,good in reproducibility,and has no interference on target components and clear spots.2.Optimization of Assay Method of Naringin Content in Zhulingjianpi Capsules In this experiment,the factors including the extraction method,extraction solvent,extraction time and solvent volume for extracting naringin from the contents of Capsules were systematically investigated and compared,and the optimal extraction method was determined.Methodological validation was performed,including linearity and range,detection limits,repeatability,stability,accuracy and precision.Using this method,the naringin content of 6 batches of samples produced in 2017-2018 was measured.The measurement result was between 0.745 and 1.0325 mg/particle,and the average content was 0.8717 mg/particle.3.Study on Fingerprint of Zhulingjianpi Capsule In this experiment,a high-performance liquid chromatographic fingerprint method of Zhulingjianpi Capsule was established.Fifteen shared peaks were identified and six known chromatographic peaks were identified.The similarity was measured by Similarity evaluation system for chromatographic fingerprint of TCM(Version 2004A).The fingerprint similarity of each batch was between 0.988 and 0.996.The established HPLC fingerprint of Zhulingjianpi Capsule is simple and reproducible,and can be used to control the quality of Zhulingjianpi Capsule comprehensively.