一测多评法同时测定小儿金翘颗粒中7种成分的含量
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篇名: 一测多评法同时测定小儿金翘颗粒中7种成分的含量
TITLE: Simultaneous Determination of 7 Constituents in Xiao ’er Jinqiao Granules by QAMS
摘要: 目的:建立同时测定小儿金翘颗粒中7种成分含量的方法。方法:采用一测多评法(QAMS)。色谱柱为LubexKromasilC18,流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),检测波长为326nm,流速为1.0mL/min,柱温为40℃,进样量为10µL。以绿原酸为内参物,计算新绿原酸、隐绿原酸、连翘酯苷A、异绿原酸B、异绿原酸A、异绿原酸C的相对校正因子;考察不同色谱系统、色谱柱、流动相比例、流速、柱温等对相对校正因子的影响,并采用两点校正法结合相对保留时间校正法对各成分进行色谱峰定位。分别按QAMS法和标准曲线法检测7种成分的含量,并进行比较。结果:新绿原酸、绿原酸、隐绿原酸、连翘酯苷A、异绿原酸B、异绿原酸A、异绿原酸C检测质量浓度的线性范围分别为9.27~92.70、37.36~373.60、13.02~130.20、7.15~71.50、4.56~45.60、6.32~63.20、14.69~146.90µg/mL(r≥0.9997);定量限分别为1.38、1.41、1.40、1.99、1.10、1.17、1.10ng,检测限分别为0.41、0.42、0.42、0.60、0.33、0.35、0.33ng;精密度、重复性、稳定性试验的RSD均小于2%,平均加样回收率为98.28%~99.15%(RSD<2%,n=9)。新绿原酸、隐绿原酸、连翘酯苷A、异绿原酸B、异绿原酸A、异绿原酸C相对于绿原酸的相对校正因子分别为0.995、1.007、0.580、1.243、1.252、1.247;不同色谱条件下其相对校正因子的RSD均小于3%。采用两点校正法结合相对保留时间校正法预测的各待测成分的保留时间与实测值的相对误差绝对值均小于2%。QAMS法测得的含量分别为2.790~3.416、14.526~17.907、3.763~4.531、1.625~1.982、1.087~1.523、1.434~2.219、3.631~5.078mg/g,标准曲线法测得的含量分别为2.811~3.438、14.512~17.893、3.739~4.508、1.656~2.012、1.108~1.544、1.460~2.245、3.597~5.045mg/g;两种方法测得含量的相对误差均在±2%以内。结论:两点校正法结合相对保留时间校正法能准确定位各成分色谱峰;所建QAMS简便、快捷、准确、可靠,可用于同时测定小儿金翘颗粒中7种成分的含量。
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.
期刊: 2020年第31卷第10期
作者: 梁欣雨,周晓钢,何兵,杨世艳
AUTHORS: LIANG Xinyu,ZHOU Xiaogang ,HE Bing,YANG Shiyan
关键字: 一测多评法;小儿金翘颗粒;含量测定;色谱峰定位;两点校正法;相对保留时间校正法
KEYWORDS: QAMS;Xiao’er jinqiao granules ;Content determination ;Peak location ;Two-point correction method ;Relative
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