摘要
功效成分是保健食品常见的一项检测项目,是控制保健食品质量的重要指标。本文建立了超高效液相色谱-串联质谱同时测定保健食品中14种功效成分的快速检测方法。样品前期采用甲醇超声提取,采用Venusil MP C18(100 mm×2.1 mm,3μm)色谱柱,0.1%甲酸水-乙腈为流动相,梯度分离后使用串联四级杆质谱进行检测,外标法峰面积进行定量。结果表明,超高效液相色谱-串联质谱的方法能在4 min内完成所有样品的出峰。芦荟苷、腺苷在0.05~10 ng/mL,芦丁、淫羊藿苷、苦杏仁苷、芍药苷在0.5~100 ng/mL,其余8种功效成分在5~1000 ng/mL浓度范围内线性关系良好(r>0.998)。方法精密度相对标准偏差<5%。绿原酸、没食子酸、丹参素钠、白藜芦醇、红景天苷、黄氏甲苷、甘草酸、大蒜素检出限为75μg/kg,芦荟苷、腺苷检出限为0.75μg/kg,芦丁、淫羊藿苷、苦杏仁苷、芍药苷检出限为7.5μg/kg。通过三个浓度的加标回收实验表明,方法回收率在83.42%~108.44%。该方法灵敏度高、线性关系和重现性好,可快速地对保健食品中多种植物功效成分进行同时测定,可为保健食品的质量监控提供一定的技术参考。
The functional component and composition are commonly analyzed for health foods,and are important quality indices of these products.An ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)method was established for simultaneous determination of 14kinds of plant-based ftmctional components present in health foods.Ultrasonic extraction with methanol was applied to the samples prior to analysis by UPLC-MS/MS using a Venusil MP C18column (100mm×2.1mm,3μm)and a gradient mobile phase composed of acetonitrile and water containing 0.1%formic acid.The chromatographic peak areas were quantified using external standards.The results showed that the chromatographic peak of all the test samples were eluted within 4min by the present UPLC-MS/MS method.Good linearity was observed in the range of 0.05-10ng/mL for aloin and adenosine,0.5-100ng/mL for rutin,icariin, amygdalin and paeonlflorin,and 5-1000ng/mL for the other 8kinds of functional components,with the correlation coefficients greater than 0.998.The method precision,the relative standard deviation,was less than 5%.The detection limit was 75μg/kg for chlorogenlc acid,gallic acid,sodium danshensu,resveratrol,salidroside,astragaloside,glycyrrhizin and allicin,0.75μg/kg for aloin and adenosine,and 7.5μg/kg for turin,icariin,amygdalin and paeoniflorin.The recovery rate was 83.42%-108.44%based on the recoveries of the spike-and-recovery experiments at three standard concentrations.Thus,this current method had a high sensitivity,good linear relationship and reproducibility, and can be used for simultaneous determination of various functional components in a health food,which provides a technical support for the quality control of health foods.
作者
杨惠成
王海鸣
林绪
燕云
何晓峰
YANG Hui-cheng;WANG Hai-ming;LIN Xu;YAN Yun;HE Xiao-feng(Guangzhou Grg Metrology &Test Co.,Ltd,Guangzhou 510065)
出处
《现代食品科技》
EI
CAS
北大核心
2018年第11期281-289,20,共10页
Modern Food Science and Technology
关键词
保健食品
植物功效成分
超高效液相色谱-串联质谱
health food
plant-based functional components
ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)