Wang Ya-Dan, He Yi, Dai Zhong, Ma Shuang-Cheng
National Institutes for Food and Drug Control, Beijing 100050, China.
Zhongguo Zhong Yao Za Zhi. 2016 May;41(10):1870-1875. doi: 10.4268/cjcmm20161018.
In this study, an HPLC-MS/MS method was developed and validated for simultaneous determination of six iridoids and four flavonoids in batches of Lonicerae Flos samples. Chromatographic separation was performed on a Shiseido Capcell Pak-C₁₈ column (4.6 mm×250 mm, 5 μm). 0.1% Aqueous formic and acid (A) and acetonitrile (B) were adopted as mobile phase. Detection was carried out on a triple quadrupole mass spectrometer in the negative ion mode using an electrospray source. Multiple reaction monitoring (MRM) mode was employed. The developed method showed good linearity (R² ≥0.999 0) for all the analytes within the test ranges and the limits of quantification (LOQs) ranged from 7.4 to 31.0 μg•L⁻¹. The recoveries varied between 94.16% and 105.3%. The quantitative data indicated that the total content of iridoids (0.338%-1.440%) was much higher than that of flavonoids (0.015 4%-0.057 5%) in all samples. Moreover, it was found that there were significant differences in the content of six compounds among the samples from three different original plants, which might provide scientific evidences for the origin identification and quality control of Lonicerae Flos.
本研究建立并验证了一种高效液相色谱-串联质谱法(HPLC-MS/MS),用于同时测定多批次金银花样品中的六种环烯醚萜类化合物和四种黄酮类化合物。色谱分离在资生堂Capcell Pak-C₁₈柱(4.6 mm×250 mm,5μm)上进行。采用0.1%甲酸水溶液(A)和乙腈(B)作为流动相。在配备电喷雾源的三重四极杆质谱仪上以负离子模式进行检测,采用多反应监测(MRM)模式。所建立的方法在测试范围内对所有分析物均显示出良好的线性(R²≥0.999 0),定量限(LOQs)范围为7.4至31.0μg•L⁻¹。回收率在94.16%至105.3%之间。定量数据表明,所有样品中环烯醚萜类化合物的总含量(0.338%-1.440%)远高于黄酮类化合物的总含量(0.015 4%-0.057 5%)。此外,发现来自三种不同原生植物的样品中六种化合物的含量存在显著差异,这可能为金银花的产地鉴定和质量控制提供科学依据。