Zhang Xiao, Guo Qing, Yu Boyang
Department of Complex Prescription of Traditional Chinese Medicines, China Pharmaceutical University, Nanjing, P. R. China.
Jiangsu Institute for Food and Drug Control, Nanjing, P. R. China.
J Sep Sci. 2015 Dec;38(23):4014-20. doi: 10.1002/jssc.201500917. Epub 2015 Nov 9.
Lonicerae Japonicae Flos is often adulterated with Lonicerae Flos, which is derived from the other four Lonicera species, in both the crude drug and Lonicerae Japonicae Flos preparations. We proposed a methodology for the quantitative analysis of adulterant Lonicerae Flos in Lonicerae Japonicae Flos preparations. Taking macranthoidins A, B, dipsacoside B (saponins), sweroside (iridoids), and luteolin-7-O-d-glucoside (flavonoids) as markers, a method of ultra high performance liquid chromatography with triple quadrupole mass spectrometry was employed to determine their amounts in Lonicerae Flos, Lonicerae Japonicae Flos, and Lonicerae Japonicae Flos preparations. The proportion of adulterant Lonicerae Flos in Lonicerae Japonicae Flos preparations was estimated based on the saponin contents of Lonicerae Japonicae Flos and Lonicerae Flos. All analytes separated under isocratic elution in 12 min with acceptable linearity, precision, repeatability, and accuracy. Lonicerae Japonicae Flos was easily distinguished from Lonicerae Flos by the total amount of saponins (0.067 and > 45.8 mg/g for Lonicerae Japonicae Flos and Lonicerae Flos, respectively). Eighteen of twenty one Lonicerae Japonicae Flos preparation samples were adulterated with Lonicerae Flos in proportions of 11.3-100%. The developed ultra high performance liquid chromatography with triple quadrupole mass spectrometry method could be used for the identification of Lonicerae Japonicae Flos and the four species of Lonicerae Flos and for the analysis of Lonicerae Japonicae Flos preparations adulterated with Lonicerae Flos.
金银花常与来源于其他四种忍冬属植物的忍冬花掺伪,在生药和金银花制剂中均有出现。我们提出了一种定量分析金银花制剂中掺伪忍冬花的方法。以大花忍冬苷A、B、川续断皂苷B(皂苷类)、獐牙菜苷(环烯醚萜类)和木犀草素-7-O-β-D-葡萄糖苷(黄酮类)为标志物,采用超高效液相色谱-三重四极杆质谱联用法测定忍冬花、金银花及金银花制剂中它们的含量。基于金银花和忍冬花的皂苷含量估算金银花制剂中掺伪忍冬花的比例。所有分析物在等度洗脱条件下12分钟内分离,线性、精密度、重复性和准确度良好。通过皂苷总量可轻松区分金银花和忍冬花(金银花和忍冬花的皂苷总量分别为0.067和>45.8 mg/g)。21个金银花制剂样品中有18个掺有忍冬花,掺伪比例为11.3 - 100%。所建立的超高效液相色谱-三重四极杆质谱联用法可用于金银花及四种忍冬花的鉴别,以及分析掺有忍冬花的金银花制剂。