分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2010年
2期
169-174
,共6页
朱明达%马微%陈冬东%彭涛%李淑娟%赵广华%唐英章
硃明達%馬微%陳鼕東%彭濤%李淑娟%趙廣華%唐英章
주명체%마미%진동동%팽도%리숙연%조엄화%당영장
超高效液相色谱-电喷雾串联质谱%蜂胶%活性成分%降糖西药
超高效液相色譜-電噴霧串聯質譜%蜂膠%活性成分%降糖西藥
초고효액상색보-전분무천련질보%봉효%활성성분%강당서약
Ultra performance liquid chromatography tandem mass spectrometry%Propolis%Active compounds)%Anti-diabetic drugs
采用超高效液相色谱-电喷雾串联四极杆质谱仪(UPLC-ESI-MS/MS)同时测定蜂胶保健品中14种活性成分和9种违禁降糖西药.蜂胶保健品样品用甲醇稀释,超声波提取, 样品溶液经高速离心后过滤.使用ACQUITY UPLC C_(18))反相柱(50 mm ×2.1 mm , 1.7μm);流动相为0.3%甲酸溶液和乙腈,在梯度条件下分析,目标分析物在多反应监测(MRM)模式下以保留时间和离子对(母离子和两个碎片离子)信息比较进行定性和定量分析.本方法的活性成分检出限(LOD)为0.7~42.0 mg/kg;定量限(LOQ)为2.2~140 mg/kg;活性成分的加标回收率为77.8%~113.6%;违禁降糖西药的LOD为0.1~0.9 mg/kg,LOQ为0.3~2.5 mg/kg);违禁降糖西药的平均回收率为79.3%~108.5%.本方法简便、有效、灵敏,为评价蜂胶保健品质量提供了新的检测方法.
採用超高效液相色譜-電噴霧串聯四極桿質譜儀(UPLC-ESI-MS/MS)同時測定蜂膠保健品中14種活性成分和9種違禁降糖西藥.蜂膠保健品樣品用甲醇稀釋,超聲波提取, 樣品溶液經高速離心後過濾.使用ACQUITY UPLC C_(18))反相柱(50 mm ×2.1 mm , 1.7μm);流動相為0.3%甲痠溶液和乙腈,在梯度條件下分析,目標分析物在多反應鑑測(MRM)模式下以保留時間和離子對(母離子和兩箇碎片離子)信息比較進行定性和定量分析.本方法的活性成分檢齣限(LOD)為0.7~42.0 mg/kg;定量限(LOQ)為2.2~140 mg/kg;活性成分的加標迴收率為77.8%~113.6%;違禁降糖西藥的LOD為0.1~0.9 mg/kg,LOQ為0.3~2.5 mg/kg);違禁降糖西藥的平均迴收率為79.3%~108.5%.本方法簡便、有效、靈敏,為評價蜂膠保健品質量提供瞭新的檢測方法.
채용초고효액상색보-전분무천련사겁간질보의(UPLC-ESI-MS/MS)동시측정봉효보건품중14충활성성분화9충위금강당서약.봉효보건품양품용갑순희석,초성파제취, 양품용액경고속리심후과려.사용ACQUITY UPLC C_(18))반상주(50 mm ×2.1 mm , 1.7μm);류동상위0.3%갑산용액화을정,재제도조건하분석,목표분석물재다반응감측(MRM)모식하이보류시간화리자대(모리자화량개쇄편리자)신식비교진행정성화정량분석.본방법적활성성분검출한(LOD)위0.7~42.0 mg/kg;정량한(LOQ)위2.2~140 mg/kg;활성성분적가표회수솔위77.8%~113.6%;위금강당서약적LOD위0.1~0.9 mg/kg,LOQ위0.3~2.5 mg/kg);위금강당서약적평균회수솔위79.3%~108.5%.본방법간편、유효、령민,위평개봉효보건품질량제공료신적검측방법.
A comprehensive analytical method based on ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of active components and anti-diabetic) drugs in propolis health foods. The samples were extracted by ultrasound extraction with methanol). The insoluble residue of extract was removed by freeze-centrifuging. The analysis was performed on an ACQUITY UPLC C_(18)) column(50 mm ×1 mm, i.d., 1.7 μm) utilizing a gradient elution profile and a mobile phase of 0.3% formic acid in water and acetonitrile. The analytes were detected using an electro spray ionization tandem mass spectrometry with multiple reaction monitoring. Qualitative and quantitative analysis was based on the peak area of the parent ion and two fragment ions. The LOD and LOQ level for 14 active components ranged from 0.7 mg/kg to 42.0 mg/kg and 2.2 mg/kg to 140 mg/kg respectively, and recoveries were 77.8%-113.6%, with the intra- and inter-day precision less than 15%. The LOD and LOQ level for 9 anti-diabetics) ranged from 0.1 mg/kg to 0.9 mg/kg and 0.3 mg/kg to 2.5 mg/kg respectively, and recoveries) were 79.3%-108.5%, with the intra- and inter-day precision less than 15%. The method is simple) and sensitive, and can be used for quality control of propolis.