Objective: To establish an accelerated solvent extraction(ASE)-HPLC method to determine chrysophanol and aurantio-obtusin in Cassia obtusifolia L.Methods: The optimal extraction conditions were defined by orthogonal tests using ASE.The method was carried out on an ACE Excel C18-PFP column (75 mm×2.1 mm,2.5 μm) with the mobile phase consisting of 0.1% phosphoric acid solution-acetonitrile with gradient elution.The column temperature was 40 ℃,the flow rate was 0.4 ml·min-1, and the detection wavelength was 284 nm. Results: The best process parameters of ASE were as follows:the extraction solvent was methanol, the extraction temperature was 120 ℃ and the static extraction duration was 5 minutes for three cycles.The ASE method needed only 1/9 of the time as the pharmacopoeia method,while the extraction efficiency of the ASE method was higher.The linear ranges of cassia obtusifolia L.and Chrysophanol were at 0.73~58.57 μg·ml-1(r=0.999 7) and 1.09~87.29 μg·ml-1(r=0.999 6).The average recoveries were 102.7%(RSD=0.8%) and 98.2%(RSD=1.5%).Conclusion: The method is simple, rapid and sensitive, which can be used for the rapid determination of aurantio obtusin and chrysophanol in Cassia obtusifolia L.

At present, drug safety has gradually become the focus of world attention, and the study and control of related sub-stances is one of the key elements for drug safety. The national drug standards are also gradually increased the control requirements for related substances. Therefore, the detection and control of related substances are extremely important in the safety of drugs. By summa-rizing the analysis methods for related substances in drugsand their application , the paper alms to provide references for quality control of drugs.

OBJECTIVETo develop a method for the simultaneous determination of aflatoxin B1, B2, G1, G2 and ochratoxin A in Glycyrrhiza uralensis by HPLC-FLD after immunoaffinity column with online post-column photochemical derivatization.

METHODSample was extracted with MeOH: H2O (80:20) and cleaned up by immunoaffinity column. The toxins were separated by reversed-phase HPLC and the mobile phase was consisted of methanol and 0.5% acetic acid solution with gradient elution. The determination was carried out by fluorescence detector after photochemical derivatization.

RESULTThe detection limits of aflatoxin G2, G1, B2, B1 and ochratoxin A were 0.02, 0.06, 0.015, 0.03 and 0.25 microg x kg(-1), respectively. The recoveries of analytes were from 76.0% to 103% and the relative standard deviations (RSDs) were below 13%.

CONCLUSIONThe method is a simple, accurate and can be used to determine the contents of aflatoxin B1, B2, G1, G2 and ochratoxin A in G. uralensis simultaneously.

Aflatoxins ; chemistry ; isolation & purification ; Chromatography, Affinity ; methods ; Chromatography, High Pressure Liquid ; methods ; Glycyrrhiza uralensis ; chemistry ; Ochratoxins ; chemistry ; isolation & purification ; Photochemical Processes

Objective: To establish a method for the simultaneous determination of four chromones in Saposhnikoviae Radix by multi-components with single marker ( QAMS) .Methods:An HPLC analysis was used to determine the contents of 4′-O-β-D-glucosyl-5-O-methylvisamminol , cimifugin and sec-O-glucosylhamaudol in Saposhnikoviae Radix.Prim-O-glucosylcimifugin was chosen as the single maker.The contents of 4 chromones in 10 batches of samples were determined by both external standard method and QAMS .The reliability and feasibility of the method were evaluated by the comparison of the quantitative results between the external standard meth -od and QAMS.Results:The relative correction factor (RCF) was perfect.The results calculated by the single marker were consistent with the results from the external standard method .Conclusion:The method with single marker is accurate and feasible to evaluate the quality of Saposhnikoviae Radix.