超高效液相色谱-串联质谱测定葫芦瓜中葫芦素E和葫芦素E-2-O-beta-D-葡萄糖苷

Determination of cucurbitacin E and cucurbitacin E-2-O-beta-D-glucoside in gourd melon by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  HLB固相萃取  超高效液相色谱-串联质谱  葫芦瓜  葫芦素E和葫芦素E-2-O-beta-D-葡萄糖苷

英文关键词:HLB extraction  ultra performance liquid chromatography-tandem mass spectrometry  gourd melon  cucurbitacin E and cucurbitacin E-2-O-beta-D-glucoside

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定葫芦瓜中葫芦素E和葫芦素E-2-O-beta-D-葡萄糖苷含量的方法。方法 样品以甲醇重复提取后, 旋转蒸发浓缩, 经HLB固相萃取柱净化。在优化后的仪器条件下, 采用电喷雾电离(electron spray ionization, ESI)负离子模式进行电离, 并通过多反应监测(multi-selected reaction monitoring, MRM)模式采集目标化合物的离子参数。结果 葫芦素E和葫芦素E-2-O-beta-D-葡萄糖苷在一定浓度范围内线性良好, 相关系数r分别为0.9998和0.9995, 平均回收率范围为80.4%~91.8%, 相对标准偏差为3.98%~6.21%, 方法检出限(limit of detection, LOD)为10.0和2.0 μg/kg。结论 该方法操作简单便捷, 成本低, 回收率高, 灵敏度高, 重现性好, 适合用于测定葫芦瓜中葫芦素E和葫芦素E-2-O-beta-D-葡萄糖苷的含量。

英文摘要:

      Objective To establish a method of determination of cucurbitacin E and cucurbitacin E-2-O-beta-D-glucoside in gourd melon by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After being extracted repeatedly by methanol, the supernatant was rotary evaporated and purified by HLB solid phase extraction column. The samples were determined by UPLC-MS/MS under the negative electrospray ionization mode of electron spray ionization (ESI) with the optimized conditions. The ion parameters were acquired by multi-selected reaction monitoring (MRM) scanning detection. Results The cucurbitacin E and cucurbitacin E-2-O-beta-D-glucoside showed a good linearity in a certain concentration range, with correlation coefficients of 0.9998 and 0.9995, respectively. The average recoveries ranged from 80.4% to 91.8% in the standard addition test, while the relative standard deviations (RSDs) were in the range from 3.98% to 6.21%. The limits of detection (LOD) of cucurbitacin E and cucurbitacin E-2-O-beta-D-glucoside were 10.0 and 2.0 μg/kg. Conclusion The method is simple and convenient to operate, low in cost, high in recovery rate, high in sensitivity and good in reproducibility, which is suitable for determining the content of cucurbitacin E and cucurbitacin E-2-O-beta-D-glucoside in gourd melon.