超高效液相色谱串联质谱法测定酒和功能饮料中3种西地那非衍生物的含量
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摘要
目的建立超高效液相色谱串联质谱法(ultra performance liquid chromatography tandemmass spectrometry,UPLC-MS/MS)测定酒和功能饮料中3种西地那非衍生物(N-去甲基西地那非、吡唑N-去甲基西地那非、异丁基西地那非)含量的分析方法。方法采用Agilent Eclipse Plus C18 (3.0 mm×150 mm, 1.8μm)反相色谱柱,0.1%甲酸水和0.1%甲酸乙腈为流动相,梯度洗脱,采用多反应监测(multiplereaction monitoring,MRM)检测。结果在50～500 ng/mL的浓度范围内, N-去甲基西地那非、吡唑N-去甲基西地那非、异丁基西地那非均表现出良好的线性关系,本方法中3种化合物的检出限(limit of detection, LOD)均为15 ng/mL,定量限(limit of quantitation, LOQ)均为50 ng/mL。结论该方法操作简便,结果可靠,灵敏度高,可用于酒和功能饮料中N-去甲基西地那非、吡唑N-去甲基西地那非、异丁基西地那非含量的快速测定。
Objective To establish a method for determination of 3 kinds of sildenafil derivatives(N-desmethyl sildenafil,pyrazole N-desmethyl sildenafil,and isobutyl sildenafil) in wine and functional drinks by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).Method The samples were separated on a Agilent Eclipse Plus C18(3.0 mm×150 mm,1.8 μm) using 0.1% formic acid solution and 0.1% formic acid acetonitrile as mobile phase with the gradient elution.The samples were determined by multiple reaction monitoring(MRM).Results In the concentration range of 50-500 ng/mL,N-desmethyl sildenafil,pyrazole N-desmethyl sildenafil,and isobutyl sildenafil all showed a good linear relationship.The limits of detection(LODs) of the 3 compounds were 15 ng/mL,and limits of quantitation(LOQs) were 50 ng/mL.Conclusion This method is simple,reproducible and with high sensitivity,which is suitable for the rapid analysis of N-desmethyl sildenafil,pyrazole N-desmethyl sildenafil,and isobutyl sildenafil in wine and functional drinks.
Objective To establish a method for determination of 3 kinds of sildenafil derivatives(N-desmethyl sildenafil,pyrazole N-desmethyl sildenafil,and isobutyl sildenafil) in wine and functional drinks by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).Method The samples were separated on a Agilent Eclipse Plus C18(3.0 mm×150 mm,1.8 μm) using 0.1% formic acid solution and 0.1% formic acid acetonitrile as mobile phase with the gradient elution.The samples were determined by multiple reaction monitoring(MRM).Results In the concentration range of 50-500 ng/mL,N-desmethyl sildenafil,pyrazole N-desmethyl sildenafil,and isobutyl sildenafil all showed a good linear relationship.The limits of detection(LODs) of the 3 compounds were 15 ng/mL,and limits of quantitation(LOQs) were 50 ng/mL.Conclusion This method is simple,reproducible and with high sensitivity,which is suitable for the rapid analysis of N-desmethyl sildenafil,pyrazole N-desmethyl sildenafil,and isobutyl sildenafil in wine and functional drinks.
引文
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[14]王一红,冯家力,潘振球,等.液相色谱-质谱-质谱方法同时测定抗疲劳保健食品中伐地那非、西地那非、他达那非[J].中华预防医学杂志,2009,43(8):727-729.Wang YH,Feng JL,Pan ZQ,et al.Simultaneous determination of vardenafil,sildenafil and Tadanafil in anti-fatigue health food by liquid chromatography-mass spectrometry[J].Chin J Prev Med,2009,43(8):727-729.
[15]Liew KB,Loh GO,Tan YT,et al.Simultaneous quantification of sildenafil and N-desmethyl sildenafil in human plasma by UFLC coupled with ESI-MS/MS and pharmacokinetic and bioequivalence studies in Malay population[J].Biomed Chromatogr,2015,29(6):953-960.
[16]陈聪,向平,沈保华,等.体液中西地那非的测定及其代谢物的确认[J].分析化学,2011,39(7):1093-1099.Chen C,Xiang P,Shen BH,et al.Determination of sildenafil in human blood and confirmation ofits metabolites in urine[J].Chin J Anal Chem,2011,39(7):1093-1099.
[2]Zou P,Hou P,Oh SSY,et al.Isolation and identification of thiohomosildenafil and thiosildenafil in health supplements[J].J Pharm Biomed Anal,2008,(47):279-284.
[3]Zhao L,Mason NA,Morrell NW,et al.Sildenafil inhibits hypoxia-induced pulmonary hypertension[J].Circulation,2001,104(4):424.
[4]李萍,杨金易,张燕,等.保健食品中西地那非检测方法的研究进展[J].食品安全质量检测学报,2012,3(6):705-709.Li P,Yang JY,Zhang Y,et al.Research progress on detection of sildenafil in health care food[J].J Food Saf Qual,2012,3(6):705-709.
[5]李锐,陈国彪.UPLC-Q-TOF-MS法快速检测补肾壮阳类中成药中11个PDE5型抑制剂类药物[J].药物分析杂志,2014,34(5):879-884.Li R,Chen GB.Simultaneous determination of 11 phosphodiesterase-5inhibitorsadded illegally in Chinese medicine preparations for invigorants by UPLC-Q-TOF-MS[J].Chin J Pharm Anal,2014,34(5):879-884.
[6]李航,陈小泉,杜钢,等.保健食品中11种西地那非类药物的检测[J].生命科学仪器,2014,12(3):39-44.Li H,Chen XQ,Du G,et al.Detection of 11 sildenafil drugs in health food[J].J Lif Sci Instr,2014,12(3):39-44.
[7]于泓,胡青,张甦,等.补肾壮阳类中药及保健食品中31种5型磷酸二酯酶抑制剂的高分辨四级杆飞行时间质谱定性定量检测方法[J].中国药学杂志,2013,48(15):1312-1318.Yu H,Hu Q,Zhang S,et al.Qualitative and quantitative analysis of 31PDE-5 inhibitors in herbal products and dietary supplements by UPLC/Q-TOF-MS[J].Chin Pharm J,2013,48(15):1312-1318.
[8]陈国章.HPLC法测定保健品中枸橼酸西地那非[J].实用预防医学,2004,11(2):370-371.Chen GZ.Determination of sildenafil citrate in health products by HPLC[J].Pract Prev Med,2004,11(2):370-371.
[9]李润锴,薄涛.毛细管电泳法测定性保健品中的西地那非[J].色谱,2002,20(4):335-337.Li RK,Bo T.Determination of sildenafil in sex health products by capillary electrophoresis[J].Chin J Chromatogr,2002,20(4):335-337.
[10]鲁琳,高燕红,李少霞,等.高效液相色谱-二极管阵列检测法测定保健食品中枸橼酸西地那非的研究[J].中国卫生检验杂志,2005,15(9):1052-1054.Lu L,Gao YH,Li SX,et al.Determination of sildenafil citrate in health food by high performance liquid chromatography with diode array detector[J].Chin J Health Lab Technol,2005,15(9):1052-1054.
[11]魏晓舒.HPLC测定保健品中西地那非的含量[J].华西药学杂志,2004,19(2):144-145.Wei XS.Determination of the content of Western medicine in healthy products by HPLC[J].West Chin J Ourn Pharm Sci,2004,19(2):144-145.
[12]Quintero A,Caldera A,Milano B,et al.Validation of an HPLC method for sildenafil citrate analysis in human plasma samples[J].Pharmazie,2009,64(12):796-799.
[13]张丽媛,颜琳琦,周明昊,等.高效液相色谱-串联质谱检测保健酒中非法添加物艾地那非[J].食品科学,2016,(14):198-202.Zhang LY,Yan LQ,Zhou MH,et al.Determination of aildenafil illegally added in health wine by high performance liquid chromatography tandem mass spectrometry[J].Food Sci,2016,(14):198-202.
[14]王一红,冯家力,潘振球,等.液相色谱-质谱-质谱方法同时测定抗疲劳保健食品中伐地那非、西地那非、他达那非[J].中华预防医学杂志,2009,43(8):727-729.Wang YH,Feng JL,Pan ZQ,et al.Simultaneous determination of vardenafil,sildenafil and Tadanafil in anti-fatigue health food by liquid chromatography-mass spectrometry[J].Chin J Prev Med,2009,43(8):727-729.
[15]Liew KB,Loh GO,Tan YT,et al.Simultaneous quantification of sildenafil and N-desmethyl sildenafil in human plasma by UFLC coupled with ESI-MS/MS and pharmacokinetic and bioequivalence studies in Malay population[J].Biomed Chromatogr,2015,29(6):953-960.
[16]陈聪,向平,沈保华,等.体液中西地那非的测定及其代谢物的确认[J].分析化学,2011,39(7):1093-1099.Chen C,Xiang P,Shen BH,et al.Determination of sildenafil in human blood and confirmation ofits metabolites in urine[J].Chin J Anal Chem,2011,39(7):1093-1099.