Simultaneous Determination of 7 Constituents in Xiao ’er Jinqiao Granules by QAMS / 中国药房

ABSTRACT

OBJECTIVE：To e stablish a method for simultaneous determination of 7 constituents in Xiao ’er jinqiao granules . METHODS：QAMS method was adopted. The determination was performed on Lubex Kromasil C 18 column with mobile phase consisted of acetonitrile- 0.1％ phosphoric acid solution （gradient elution ）. The detection wavelength was set at 326 nm，the flow rate was 1.0 mL/min. The column temperature was 40 ℃，and sample size was 10 µL. Using chlorogenic acid as the internal reference，the relative correction factors （RCF）of neochlorogenic acid ，cryptochlorogenic acid ，forsythiaside A ，isochlorogenic acid B ，isochlorogenic acid A and isochlorogenic acid C were calculated. The effects of different chromatogram system ， chromatogram column ，the ratio of mobile phase ，flow rate and column temperature on RCF were investigaten. According to the two-point correction method combined with the relative retention time correction of the components to be tested ，the peak location was carried out. The contents of 7 components were determined by QAMS and SCM respectively and then compared. RESULTS： The linear range of neochlorogenic acid ，chlorogenic acid ，cryptochlorogenic acid ，forsythoside A ，isochlorogenic acid B ，isochlorogenic acid A ，isochlorogenic acid C were 9.27-92.70，37.36-373.60，13.02-130.20，7.15-71.50，4.56-45.60，6.32-63.20，14.69-146.90 µg/mL （r≥0.999 7）. The limits of quantification were 1.38，1.41，1.40，1.99，1.10，1.17，1.10 ng，respectively；and the limits of detection were 0.41，0.42，0.42，0.60，0.33，0.35，0.33 ng，respectively. RSDs of precision ，repeatability and stability tests were all less than 2％；average recoveries were 98.28％-99.15％ （RSD＜2.0％ ， n＝9）. RCFs of neochlorogenic acid ， （No.2013LZLY-K61） cryptochlorogenic acid ，forsythiaside A ，isochlorogenic acid B，isochlorogenic acid A and isochlorogenic acid C relative to xinyuliang@stu.cqmu.edu.cn chlorogenic acid were 0.995，1.007，0.580，1.243，1.252 and 1.247，respectively. RSDs of RCFs were all lower than 3％ under different chromatogram conditions. Absolute value of relative error between the relative retention time of components to be tested predicted by two-point correction combined with relative retention time correction and measured value was less than 2％. The contents measured by QAMS were 2.790-3.416， 14.526-17.907，3.763-4.531，1.625-1.982，1.087-1.523，1.434-2.219，3.631-5.078 mg/g；the contents measured by SCM method were 2.811-3.438，14.512-17.893，3.739-4.508，1.656-2.012，1.108-1.544，1.460-2.245，3.597-5.045 mg/g；relative errors of the two methods were within ±2％. CONCLUSIONS ：Two-point correction method combined with relative retention time correction can accurately locate the peaks of each constituent ；established QAMS method is simple ，rapid，accurate and reliable ，it can be used for simultaneous determination of 7 constituents in Xiao ’er jinqiao granules.