摘要
目的建立一种简单、快速、灵敏、准确地鉴定中药制剂中是否添加西地那非的高效液相色谱串联质谱(LC/MS/MS)的分析方法。方法样品经C18(4.6mm×250mm,5μm),流速200μL·min-1,乙腈-0.05mol·L-1乙酸铵(1:1)流动相进行分离。在ESI正离子采集模式下,采用LC/MS/MS的多反应监测(MRM)对西地那非进行定量监测,采用外标法定量。结果本方法满足分析要求,并对12种市场上中药中西地那非进行定量测定。结论目前市场中药制剂中存在添加西地那非的现象。
Abstract
OBJECTIVE A method of HPLC/MS/MS was developed for the identification of sildenafil added in Chinese traditional medicines.METHODS HPLC Separation was carried out on a C18(4.6 mm×250 mm,5 μm) column using an isocratic mobile phase with the flow rate 200 μL·min-1.Detection is performed on API 3000 LC/MS/MS system with ESI resources in positive ion acquisition mode and qualified in multiple reaction monitoring(MRM) mode.RESULTS This method is simple,rapid,sensitive and reliable and has been successfully applied to identify sildenafil in 12 kinds of related Chinese traditional medicines.CONCLUSION Sildenafil were added in some Chinese traditional medicines.
关键词
高效液相色谱串联质谱 /
西地那非 /
中药
{{custom_keyword}} /
Key words
HPLC/MS/MS /
sildenafil /
Chinese traditional medicines
{{custom_keyword}} /
左海根;占春瑞;罗晓洪.
高效液相色谱-串联质谱法测定中药制剂中西地那非的含量[J]. 中国药学杂志, 2008, 43(07): 541-543
ZUO Hi-gen;ZHN Chun-rui;LUO Xio-hong.
Determination of Sildenafil in Traditional Chinese Medicines by HPLC/MS/MS [J]. Chinese Pharmaceutical Journal, 2008, 43(07): 541-543
{{custom_sec.title}}
{{custom_sec.title}}
{{custom_sec.content}}
参考文献
[1] CHEN B， ZHU X L， YAO S Z. Analysis of sildenafil and cialis in health foods by high performance liquid chromatography/mass spectrometry[J] .Chin J Food Hygiene(中国食品卫生杂志)，2004，16 (2)：335-337.
[2] ZOU P， YIN S S， HOU P L，et al. Simultaneous determination of synthetic phosphodiesterase -5 inhibitors found in a dietary supplement and pre-mixed bulk powders for dietary supplements using high-performance liquid chromatography with diode array detection and liquid chromatograph-electrospray ionization tandem mass spectrometry[J] .J Chromatogr B，2006，1104：113-122.
[3] LI R K， BO T， LIU H W，et al. Determination of sildenafil in medicines for erectile dysfunction by capillary electrophoresis [J] . Chin J Chromatogr(色谱)， 2002，20(4)：335-337.
[4] YANG D Z ，HANG H H. Determination of sildenafil citrate by HPLC [J] .Med J Chin PLA（解放军医学杂志）， 2002， 18(4)：235-236.
[5] MIAO Y S， LI W N， NI T，et al. Determination of sildenafil citrate and its related compound in tablet by RP-HPLC[J] .J China Pharm Univ（中国药科大学学报）， 2001，32(4)：273-275.
[6] TRACQUI A， LUDES B. HPLC-MS for the determination of sildenafil citrate (viagra) in biological fluids. Application to the salivary excretion of sildenafil after oral intake [J ] .J Anal Toxicol， 2003，27：88-94.
[7] YANG C D， SONG L H， MAO L H，et al. Analytical method for the determination of chloramphenicol residues in shrimps[J] . Chin J Anal Chem（分析化学）， 2004， 32(7)：905-907.
[8] XU Y J，XU G P. Determination of apomorphine， sildenafil and alprostadil in medicines for erectile dysfunction by high performance liquid chromatography-mass spectrometry[J] .Chin J Chromatogr（色谱），2005，23(6)：633-635.
{{custom_fnGroup.title_cn}}
脚注
{{custom_fn.content}}
