1.Content Determination of Paeoniflorin in Bailing Tablet by HPLC and Its Uncertainty Evaluation
Jianming LI ; Huichan HOU ; Lihong GU
China Pharmacy 2015;26(36):5152-5154
OBJECTIVE:To establish a method to determinate the content of paeoniflorin in Bailing tablet,and to evaluate the uncertainty of results. METHODS:HPLC was performed on the column of Platisil C18 with mobile phase of water- acetonitrile(87:13,V/V) at a flow rate of 1 ml/min,the detection wavelength was 230 nm,the column temperature was 25 ℃ and the injection volume was 10 μl. Quantitative analysis was conducted for the processes and procedures and the uncertainty was evaluated. RESULTS:The linear range of paeoniflorin was 0.100 1-2.502 8 μg;RSDs of precision,stability and reproducibility tests were lower than 2.0%,recovery rate was 98.7%-100.9%(RSD=0.86%,n=6). Reference substance amount,elution produce and the accuracy of method had great effect on the uncertainty. CONCLUSIONS:The established method can be used for the content determination of paeoniflorin in Bailing tablet,and the uncertainty evaluation provides reliability for the method.
2.Quality Control of Calculus Bovis in Houzao Niuhuang Powder
Huichan HOU ; Jie WANG ; Lihong GU
Traditional Chinese Drug Research & Clinical Pharmacology 1993;0(02):-
Objective To make a qualitative and a quantitative control on the Calculus Bovis in Houzao Niuhuang Powder.Methods Hyodeoxycholic acid and bilirubin in Calculus Bovis were separately identified by TLC,and the cholic acid content was determined by TLCS with the scan wavelength of ?s=380 nm,?R=650 nm.Results TLC can be used for the identification in-vitro cultured Calculus Bovis and artificial Calulus Bovis,the samples containing cultured Calulus Bovis showed the specific spots of bilirubin but no hyodeoxycholic acid spot while the samples containing artifical Calulus Bovis showed the hyodeoxycholic acid spot but no bilirubin spot.TLC-scanning can be used to measure the quantity of cholic acid,with the linear range being 0.2~1.8 ?g,average recovery rate of 99.5 %,and RSD being 3.3 %(n=6),and the results accorded with the criterion of the cultured Calculus Bovis in Chinese pharmacopoeia.Conclusion The methods can effectively control the quality of Calculus Bovis in Houzao Niuhuang Powder.
3.Study on Quality Standard Improvement for Compound Child Antifebrile Suppository
Simin XIE ; Jiayi CHEN ; Yingzhan TANG ; Lihong GU ; Jianming LI ; Huichan HOU
China Pharmacy 2020;31(17):2106-2111
OBJECTIVE:To improve the quality standard of Compound child antifebrile suppository. METHODS :Based on the previous quality standard ,TLC identification methods were established for artificial cow-bezoar and Baphicacanthis Cusiae Rhizoma et Radix. HPLC method was established for content determination of choleic acid (CA),hyodeoxycholic acid (HDCA) and paracetamol. RESULTS :TLC chromatogram of artificial cow-bezoar and Baphicacanthis Cusiae Rhizoma et Radix all showed the same color spots in the same position as the corresponding substance control or reference medicinal material ,while the negative samples had no interference. HPLC was performed on Welch Xtimate C 18 column(CA,HDCA)or Agilent ZORBAX SB-C 18 column(paracetamol)with mobile phase consisted of acetonitrile-0.5% formic acetic acid (by gradient elution ,CA and HDCA )or methanol-water(20∶80,V/V,paracetamol)at the flow rate of 1.0 mL/min. ELSD was used with a nitrogen flow-rate of 2.0 L/min at a drift tube temperature of 105 ℃(CA,HDCA). The detection wavelength was set at 244 nm(paracetamol). The linear ranges of CA,HDCA,paracetamol were 0.150 0-4.500 0,0.212 5-6.375 0,0.081 9-1.638 5 μg(all r>0.999 2). RSDs of precision , reproducibility and stability tests were all lower than 3%(n=6 or n=7). The average recoveries were 100.35%,101.39%, 98.81%(all RSD <3%,n=6). CONCLUSIONS :Based on previous quality standard of Compound child antifebrile suppository , TLC method is used to identify artificial cow-bezoar and Baphicacanthis Cusiae Rhizoma et Radix ,and the contents of CA ,HDCA and paracetamol are determined by HPLC ,which can effectively improve the quality control standard of the preparation.
4.Establishment of the method for the content determination of patulin in Citri Grandis Exocarpium
Simin XIE ; Junfei CHEN ; Huichan HOU ; Lihong GU ; Jianming LI ; Yanhui WANG
China Pharmacy 2022;33(23):2936-2939
OBJECTIVE To establish a method for the content determination of patulin in Citri Grandis Exocarpium. METHODS High-performance liquid chromatography-triple quadrupole mass spectrometer(HPLC-MS/MS)was used for the analysis. After water-soluble dispersion and pectinase enzymolysis, the Citri Grandis Exocarpium sample was extracted by acetonitrile with high-speed homogenated. The extracted solution was conducted dispersive solid phase extraction by mixing powder of MgSO4 and NaAC (4∶1,m/m),then purified on SHIMSEN 228 solid phase purification column. Water acetonitrile was used as mobile phase, and the Shim-pack XR-ODS column was used to separate the target compound. And it was detected by electrospray ionization in the negative mode under multiple reaction monitoring, and quantified by the external standard method with matrix- matched standard correction curves. RESULTS Patulin showed good linear correlation in the concentration from 5 to 200 ng/mL (r=0.999 6). RSDs of precision, reproducibility and stability tests (12 h) were all lower than 6%. The average recoveries at low, medium, high concentrations were 83.9%, 92.08%, 92.21%, respectively (RSDs were 11.09%, 5.53%, 1.75%, respectively). The limit of quantitation was 6 μg/kg and limit of detection was 3 μg/kg. Patulin was not detected in 20 batches of samples. CONCLUSIONS Established method can be used for the rapid detection and accurate quantification of patulin in Citri Grandis Exocarpium, which can provide experimental basis and method for safety study and quality control of Citri Grandis Exocarpium.