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超高效液相色谱-电喷雾三重四极杆质谱法测定中药中马兜铃酸A和B的含量
其他题名Determination of aristolochic acids A and B in Chinese herbals and traditional Chinese patent medicines using ultra high performance liquid chromatography-triple quadrupole mass spectrometry
刘萤; 韩深; 冯骞; 王金花
来源期刊色谱
ISSN1000-8713
出版年2011
卷号29期号:11页码:1076-1081
中文摘要利用超高效液相色谱-电喷雾三重四极杆质谱仪建立了中药中马兜铃酸A和B的定性定量分析方法。选取柴胡、生甘草、桔梗、龙胆泻肝丸、消胖丸、减肥茶等14种代表性样品,用甲醇-水(70∶30,v/v)溶液加热回流提取,经Oasis MAX固相萃取柱富集净化后,在Eclipse RP HD C_(18)反相柱(150mm*2.1mm,1.8mum)上进行分离;流动相为5mmol/L乙酸铵水溶液(pH 7.5)-乙腈(75∶25,v/v)。采用电喷雾离子源正离子模式(ESI~+)和多反应监测模式(MRM)进行质谱分析。马兜铃酸A和B的线性范围分别为0.5~200mug/L和1~200mu g/L,相关系数(r~2)均大于0.995;检出限(LODs)分别为5mug/kg和7.5mug/kg;定量限(LOQs)分别为12.5mug/kg和25mug/kg。在100mug/kg和500mug/kg添加水平下,马兜铃酸A和B的回收率(n=6)范围分别为60.3%~96.4%和61.3%~94.7%,相对标准偏差均不大于10.2%。该方法灵敏度高,重复性好,操作简便,适用于中药材、饮片及中成药中马兜铃酸A和B的痕量检测。
英文摘要A method for the simultaneous determination of aristolochic acids A and B in some Chinese herbals and traditional Chinese patent medicines by ultra high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS) was developed. Fourteen samples, including Radix Bupleuri, Radix Glycyrrhizae, Radix Platycodonis, Longdanxieganwan, Xiaopangwan, Slimming Tea, etc., were extracted with methanol-water (70 ∶ 30, v/v) and purified with Oasis MAX solid-phase extraction cartridges, then analyzed on an Eclipse RP HD C_(18) column (150 mm*2.1 mm, 1.8 mu m) using 5 mmol/L ammonium acetate solution (pH 7.5)-acetonitrile (75 ∶ 25, v/v) as the mobile phase. The mass spectrometric acquisition was carried out by means of electrospray ionization in positive mode (ESI~+) with multiple reaction monitoring (MRM) method. The good linearities (r~2>0.995) were achieved within the ranges of 0.5-200 mu g/L and 1-200 mu g/L for aristolochic acids A and B, respectively. The limits of detection (LODs) were 5 mu g/kg for aristolochic A and 7.5 mu g/kg for aristolochic B, and the limits of quantification (LOQs) were 12.5 mu g/kg and 25 mu g/kg, respectively. The recoveries of aristolochic acids A and B at the spiked levels of 100 mu g/kg and 500 mu g/kg ranged from 60.3% to 96.4% with the relative standard deviations (RSDs) not more than 10.2%. The results demonstrated that the proposed method is efficient, sensitive, reproducible, reliable and suitable for the trace determination of aristolochic acids A and B in Chinese herbals and traditional Chinese patent medicines.
中文关键词超高效液相色谱-串联质谱 ; 固相萃取 ; 马兜铃酸 ; 中药
英文关键词ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) solid-phase extraction (SPE) aristolochic acid traditional Chinese medicine
语种中文
国家中国
收录类别CSCD
WOS类目CHEMISTRY ANALYTICAL
WOS研究方向Chemistry
CSCD记录号CSCD:4380785
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/226850
作者单位北京出入境检验检疫局检验检疫技术中心, 北京 100026, 中国
推荐引用方式
GB/T 7714
刘萤,韩深,冯骞,等. 超高效液相色谱-电喷雾三重四极杆质谱法测定中药中马兜铃酸A和B的含量[J],2011,29(11):1076-1081.
APA 刘萤,韩深,冯骞,&王金花.(2011).超高效液相色谱-电喷雾三重四极杆质谱法测定中药中马兜铃酸A和B的含量.色谱,29(11),1076-1081.
MLA 刘萤,et al."超高效液相色谱-电喷雾三重四极杆质谱法测定中药中马兜铃酸A和B的含量".色谱 29.11(2011):1076-1081.
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