RESUMO
Objective: To simultaneously detect five components (phillyrin, chlorogenic acid, chlorpheniramine maleate, vitamin C and acetaminophen) in compound paracetamol vitamin C Yinqiao tablets.Methods: Using a Waters Xselect C18 column(250 mm×4.6 mm, 5 μm), the mobile phase consisted of acetonitril-0.1 mol·L-1 NaH2PO4(pH 3.0) with gradient elution at a flow rate of 1.0 ml·min-1.The detection wavelength was 230 nm and the column temperature was 35℃.Results: The linear range of vitamin C, acetaminophen, chlorogenic acid, chlorphenamine maleate and phillyrin was 0.500-200.200, 0.499-199.600, 0.501-200.100, 0.502-200.900 and 0.488-195.400 μg·ml-1(r＞0.999), respectively.The average recovery was 99.3%(RSD=1.5%), 97.8%(RSD=1.7%), 98.5%(RSD=1.1%), 97.1%(RSD=1.7%)and 99.8%(RSD=1.2%)(n=9), respectively.Conclusion: The simple and sensitive method can be applied in the quality control of compound paracetamol vitamin C Yinqiao tablets.
RESUMO
OBJECTIVE: To identify the structure of illegal additive D- (-) -isoascorbic acid in vitamin C Yinqiao tablets and to screen for it in different samples. METHODS: The separation of D- (-) - isoascorbic acid in vitamin C Yinqiao tablets was performed on a CAPCELL PAK NH2 column (4.6 mm × 250 mm, 5 μm) with mobile phase consisting acetonitrile -20 mmol · L-1 ammonium acetate (adjusted to pH 2.5 with formic acid) (60:40), the flow rate was 1.0 mL · min-1. D-(-)-isoascorbic acid was detected by diode array detector at 246 nm. Electrospray ionization (ESI) source in positive ion mode was applied for the identification with following parameters; nebulizer pressure of 220 kPa, drying gas temperature of 350°C, flow rate of 12 L · min-1, and capillary voltage of 3.5 kV. The additive D-(-)- isoascorbic acid in vitamin C Yinqiao tablets was separated and prepared by HPLC for further structure confirmation by 13C-NMR. RESULTS: The structure of the additive was elucidated by analyzing the fragment of [M + H]+ of the additive and comparing with that the reference substance. The additive was further confirmed as D-(-)- isoascorbic acid by 13C-NMR. D-(-) - isoascorbic acid was detected in 64 of 366 batch samples. CONCLUSION: The LC-MS method is accurate and sensitive, which can be used for rapid screening and identification of the illegal additive D- (-) - isoascorbic acid in vitamin C Yinqiao tablets. Copyright 2012 by the Chinese Pharmaceutical Association.
RESUMO
AIM:To establish a method of determining the content of chlorogenic acid,paracetmol,vitamin C and chlorphenamine maleate in Vitamin C Yinqiao Tablets. METHODS: The separation was performed in the C_(18) colunm with the mobile phase of methanol-acetonitril-0.02% phosphate acid(5∶10∶85).The flow rate was(1.0 mL/min) with the wavelength at 219 nm and 310 nm,the temperature of column was 35 ℃. RESULTS: The calibration curves were linear in the ranges of 0.03-0.13 ?g for chlorogenic acid,0.94-4.68 ?g for paracetmol,0.49-2.44 ?g for Vitamin C,0.01-0.05 ?g for chlorphenamine maleate,the average recoveries were not less than 98%,respectively. CONCLUSION: The method is simple,rapid and with satisfactory results.It is suitable for quality control of Vitamin C Yinqiao Tablets.