止得咳颗粒中连翘酯苷A成分鉴定及含量测定

Identification and Content Determination of Forsythiaside A in Zhideke Granules

目的建立止得咳颗粒成分的鉴定方法及测定相应成分含量的高效液相色谱(HPLC)法。方法采用超高效液相色谱-四极杆飞行时间串联质谱(UPLC-Q-TOF/MS)法,在负离子模式下采集数据,对止得咳颗粒的成分进行定性鉴别。采用高效液相色谱法测定鉴定出的成分含量,色谱柱为Phenomenex Kinetex XB-C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.2%磷酸溶液(梯度洗脱),流速为1.0 m L/min,检测波长为330 nm,柱温为30°C,进样量为10μL。结果根据质谱数据鉴定出连翘酯苷A成分。连翘酯苷A质量浓度在0.0237~0.2368 mg/m L范围内与峰面积线性关系良好(r=0.9998,n=6);精密度、稳定性、重复性试验的RSD均小于3.0%(n=6);平均加样回收率为99.14%,RSD为2.33%(n=9)。结论所建立的方法操作简便,结果准确,重复性好,可用于鉴定止得咳颗粒的成分并测定其相应成分的含量。

Objective To identify the components of Zhideke Granules and to establish a high-performance liquid chromatography(HPLC)method for the content determination of the corresponding components.Methods Ultra high-performance liquid chromatography quadrupole-time of flight tandem mass spectrometry(UPLC-Q-TOF/MS)was used to collect data in negative ion mode to qualitatively analyze the components in Zhideke Granules.HPLC method was adopted to determine the content of identified components in Zhideke Granules,the chromatographic column was Phenomenex Kinetex XB-C18 column(250 mm×4.6 mm,5μm),the mobile phase was methanol-0.2%phosphoric acid solution(gradient elution),the flow rate was 1.0 m L/min,the detection wavelength was 330 nm,the column temperature was 30°C,and the injection volume was 10μL.Results Forsythrine A was identified according to the mass spectrum data.The linear range of forsythiaside A was 0.0237-0.2368 mg/m L(r=0.9998,n=6).The RSDs of precision,stability and repeatability tests were less than 3.0%(n=6).The average recovery of forsythiaside A was 99.14%with RSD of 2.33%(n=9).Conclusion The method is simple,accurate and reproducible,which can be used for the identification and content determination of corresponding components in Zhideke Granules.