液相色谱-串联质谱法测定普通食品基质中特征性药材表征成分

Determination of the representational components in characteristic medicinal materials to typical food substrate by liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱法  特征性药材  表征成分

英文关键词:liquid chromatography-tandem mass spectrometry  characteristicmedicinal materials  representational components

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)同时测定补肾壮阳类食品及保健食品中9种补肾壮阳类功能成分的定性、定量的分析方法。方法 优化前处理方法, 分离条件和质谱参数。样品经70%甲醇超声提取, 提取液经Agilent ZORBAX Eclipse XDB-C18色谱柱 (3.0 mm×150 mm, 1.8 μm)分离, 流动相为乙腈和水(含有5 mmol/L甲酸铵溶液), 梯度洗脱, 流速为 0.5 mL/min, 以电喷雾离子源正/负2种离子多反应监测模式进行MS/MS检测。其中补骨脂素、异补骨脂素、蛇床子素以正离子模式进行检测, 淫羊藿苷、马钱苷、仙茅苷、柚皮苷、金丝桃苷、特女贞苷以负离子模式进行检测。结果 选用压片糖果和配制酒为基质, 马钱苷和金丝桃苷在20~4000 ng/mL范围内、其余7种化合物在2~400 ng/mL范围内线性关系良好, 相关系数r≥0.999。金丝桃苷和马钱苷的定量限为0.5 mg/kg, 其余7种化合物的定量限均为0.05 mg/kg。在2种基质中添加不同水平的标准溶液, 加标回收率范围在67.0%~110.5%, RSD＜10%。日内和日间精密度良好, RSD＜10%。结论 该方法能快速筛查食品及保健食品中的非药食同源补肾壮阳成分, 并为监管收集数据和提供技术支撑。

英文摘要:

      Objective To establish a method of the simultaneous determination of nine functional components in kidney-tonifying and aphrodisiac food and health food by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The pretreatment methods, separation conditions and mass spectrum parameters were optimized. The samples were ultrasonicized with 70% methanol, and the extracted solution was separated on an Agilent Zorbax Eclipse XDB-C18 column (3.0 mm×150 mm, 1.8 μm). The mobile phase was acetonitrile and water (containing 5 mmol/L ammonium formate solution). The flow rate was 0.5 mL/min. MS/MS detection was performed with positive/negative ion multi-reaction monitoring mode of electrospray ion source. Psoralen,angelicin and osthole were carried out in positive ion mode. The icariln, loganin, curculigoside, hyperoside, specnuezhenide and naringin were carried out in negative ion mode. Results The pressed candy and prepared winewas chosen as matrix, the linear range of maganin and hyperoside was 20?4000 ng/mL and the range of the other seven compounds was 2? 400 ng/mL, with the correlation coefficients r≥0.999. The limits of quantification were 0.5 mg/kg of loganin and hyperoside, and the limits of quantification were 0.05mg/kg of the other seven compounds. The average recoveries were 67.0%?110.5% when different levels of standard solution were added to the two substrates, and the relative standard deviations (RSDs) were under 10%. The intra-day and intra-day precision were good, RSD＜10%. Conclusion The method can quickly screen the non-drug food homologous kidney-tonifying and aphrodisiac ingredients in food and health food, and collect data and provide technical support for supervision.