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乐山市食品药品检验检测中心
纸质出版日期:2020,
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[1]罗华玲,朱敏凤.液质联用法测定复方板蓝根颗粒中2种成分的含量[J].西南医科大学学报,2020,43(05):456-462.
LUO Hualing, ZHU Minfeng. Determination of the content of two components in compound Radix isatidis granules by HPLC-MS/MS[J]. Journal of Southwest Medical University, 2020,43(5):456-462.
目的:建立应用液质联用(HPLC-MS/MS)法全面监测和控制复方板蓝根颗粒中原药材(板蓝根、大青叶)的投料情况
并可同时测定(R
S)-告依春、靛玉红含量的方法。方法:采用Inertsil ODS-3 (2.1×150 mm×5μm)色谱柱
柱温40℃
甲醇-0.05%甲酸(1585)的流动相等度洗脱;以HPLC分离有效成分、采用电喷雾(ESI)离子源正离子模式检测
选择多反应离子监测方式(MRM)对原药材的投料情况进行定性监测
并对有效成分进行定量分析。结果:通过分析供试品与对照药材、对照品的一级质谱图的共有特征峰
可判断供试品是按处方工艺投料;通过测定(R
S)-告依春、靛玉红两有效成分的色谱峰面积
计算出了8批次中2种成分的含量。结论:(R
S)-告依春、靛玉红分别在1.07~21.48μg/mL (r=0.999 4)
1.032~20.64μg/mL (r=0.999 5)浓度内线性关系良好;精密度试验的RSD分别为0.7%、0.5%;平均回收率分别为92.04%
90.49%。结论:该法快速简便、准确可靠、灵敏度高
适用于全面监测和控制复方板蓝根颗粒中原料药(板蓝根、大青叶)的投料情况及质量。
Objective: To develop a high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method to comprehensively monitor and control the feeding of raw medicinal materials(Radix isatidis and Folium isatidis) in compound R. isatidis granules and to determinate the content of(R
S)-goitrin and indirubin. Methods: An Inertsil ODS-3 column(2.1×150 mm × 5 μm)(column temperature: 40 °C) was used for isocratic elution with a mobile phase of methanol ~ 0.05% formic acid(15:85). Active ingredients were separated by HPLC.The determination was performed using the electrospray ionization source in positive ion mode; multiple reaction monitoring was selected for qualitative monitoring of the feeding of raw medicinal materials
and active ingredients were quantitatively analyzed. Results: Analysis of the common characteristic peaks of test article with reference herb and reference substance on the primary mass spectrum indicated that the feeding for the test article was based on the formula process. The content of(R
S)-goitrin and indirubin in 8 batches was calculated by determining the chromatographic peak areas of the two active ingredients.(R
S)-goitrin and indirubin showed a good linear relationship within the ranges of 1.07 ~ 21.48 μg/mL(r = 0.999 4) and 1.032 ~ 20.64 μg/mL(r = 0.999 5)
respectively;the relative standard deviations of precision experiments were 0.7% and 0.5%
respectively; the average recovery rates were 92.04% and 90.49%
respectively. Conclusion: The method is simple
convenient
accurate
reliable
and highly sensitive
which makes it suitable for comprehensive monitoring and control of the feeding and quality of raw medicinal materials(R. isatidis and F. isatidis) in compound R. isatidis granules.
复方板蓝根颗粒全面监测原药材液质联用
Compound Radix isatidis granuleComprehensive monitoringRaw medicinal materialHigh-performance liquid chromatography-tandem mass spectrometry
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