超高效液相色谱-串联质谱法测定减肥类保健品中的西布曲明
Determination of Sibutramine in Weight-Loss by UHPLC-MS/MS
摘 要
采用超高效液相色谱-串联质谱法测定减肥类保健品中的西布曲明.样品经甲醇超声提取后,使用Phenomenex Kinetex C18色谱柱分离,以乙腈-10 mmol·L-1乙酸铵溶液(含0.1%甲酸)为流动相进行梯度洗脱,质谱中选择多反应选择离子监测模式检测,以西布曲明-D6作为同位素内标进行定量.西布曲明的质量浓度在5.00~400 μg·L-1范围内呈线性,测定下限(10S/N)为10 ng·g-1.加标回收率在97.0%~104%之间,相对标准偏差(n=9)为1.1%~3.0%.
西布曲明
同位素内标
减肥类保健品
UHPLC-MS/MS
Sibutramine
Isotope internal standard
Weight-loss
Abstract
UHPLC-MS/MS was used for the determination of sibutramine in health products for weight-loss. The sample was extracted with methanol by ultrasonic,then separated on a Phenomenex Kinetex C18 column with the mixture of acetonitrile and 10 mmol·L-1 ammonium acetate solution containing 0.1% (φ) formic acid solution as mobile phase for gradient elution. MRM was adopted in MS detection. D6-Sibutramine was used as internal standard for quantification. The linear range for the mass concentration of sibutramine was 5.00-400 μg·L-1,and the lower limit of determination (10S/N) was 10 ng·g-1. The recovery rates measured by standard addition method were in the range of 97.0%-104%,with RSD (n=9) in the range of 1.1%-3.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201507026
所属栏目 专题报道(药物分析)
基金项目 上海市科委科研计划项目(12142201000)
收稿日期 2014/7/21
修改稿日期
网络出版日期
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备注李杰(1983-),男,甘肃兰州人,工程师,博士,研究方向为色谱-质谱联用技术研究、标准物质研制.
引用该论文: LI Jie,XU Zhuo-ni,YU Rui-xiang,LI Yong-li,CHEN Ying,WANG Hu. Determination of Sibutramine in Weight-Loss by UHPLC-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(7): 995～998
李杰,许卓妮,于瑞祥,李永利,陈鹰,王虎. 超高效液相色谱-串联质谱法测定减肥类保健品中的西布曲明[J]. 理化检验－化学分册, 2015, 51(7): 995～998
被引情况:
【1】祝伟霞,刘亚风,孙转莲,张丽,张丹, "超高效液相色谱-串联质谱法同时测定保健品中26种非法添加物",理化检验－化学分册 52, 1286-1291(2016)
【2】陈国权,雷 毅, "高效液相色谱法测定降血压类健康产品中的6种二氢吡啶类成分",理化检验－化学分册 52, 770-773(2016)
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参考文献
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【15】DING Li,HAO Xin-yu,HUANG Xin,et al.Simultaneous determination of sibutramine and its N-desmethyl metabolites in human plasma by liquid chromatography-electrospray ionization-mass spectrometry: method and clinical applications[J]. Analytica Chimica Acta,2003,492(1/2):241-248．
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【2】孙骏,赵起,李明,等.关注减肥药西布曲明的安全性[J].药学与临床研究,2010,18(2):118-119．
【3】赖天兵,胡小红,刘晓革.减肥类保健食品违禁添加药物现状及特点[J].中国食品卫生杂志,2007,19(4):336-337．
【4】秦宗会,蒲利军,谭蓉,等.盐酸西布曲明衍生光度法分析研究[J].药物分析杂志,2006,26(11):1656-1658．
【5】谢兵,庞向东,汤伟.溴酚蓝分光光度法测定盐酸西布曲明[J].理化检验-化学分册,2012,48(2):229-232．
【6】DIEFENBACH I C,FRIEDRICH M,DOS M R,et al.Development and validation of a column high-performance liquid chromatographic method for determination of sibutramine in capsules[J]. Journal of AOAC International,2009,92(1):148-151．
【7】CHANDORKAR J G,KOTWAL V B,DHANDE N S,et al.Development and validation of high performance liquid chromatography method for analysis of sibutramine hydrochloride and its impurity[J]. Pakistan Journal of Pharmaceutical Sciences,2008,21(2):121-124．
【8】朱志鑫,吴惠勤,黄晓兰,等.气相色谱-质谱法检测减肥食品中芬氟拉明和西布曲明[J].现代食品科技,2012,28(10):1419-1422．
【9】VENKATA S P,CHALLA B R,NADENDLA R.Quantication of sibutramine and its two metabolites in human plasma by LC-ESI-MSMS and its application in a bioequivalence study[J]. Journal of Pharmmaceutical Analysis,2012,2(4):249-257．
【10】ZOU P,OH S S,KIANG K H,et al.Detection of sibutramine,its two metabolites and one analogue in a herbal product for weight loss by liquid chromatography triple quadrupole mass spectrometry and time-of-flight mass spectrometry[J]. Rapid Commun. Mass Spectrom,2007,21(4):614-618．
【11】黄芳,吴惠勤,黄晓兰,等.高效液相色谱-串联质谱法同时测定保健品中非法添加的六种减肥化学品[J].分析测试学报,2007,32(6):699-704．
【12】刘卫霞,罗勇,杨维成.有机同位素稀释质谱法在食品安全分析中的应用[J].化学世界,2011,52(3):184-187．
【13】权伍英,栾燕,张欣.LC-MS/MS检测减肥保健品中的盐酸芬氟拉明和盐酸西布曲明[J].中国卫生检验杂志,2007,17(1):10-12．
【14】KANG W,BAE K,NOH K,et al.Enantioselective determination of sibutramine and its active metabolites in human plasma[J]. Journal of Pharmaceutical and Biomedical Analysis,2010,51(1):264-267．
【15】DING Li,HAO Xin-yu,HUANG Xin,et al.Simultaneous determination of sibutramine and its N-desmethyl metabolites in human plasma by liquid chromatography-electrospray ionization-mass spectrometry: method and clinical applications[J]. Analytica Chimica Acta,2003,492(1/2):241-248．
【16】CHEN Jun,LU Wei,ZHANG Qi-zhi,et al.Determination of the active metabolite of sibutramine by liquid chromatography-electrospray ionization tandem mass spectrometry[J]. Journal of Chromatography B,2003,785(2):197-203．
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