中药中掺假柠檬酸西地那非和甲基睾酮的高效液相色谱分析

Y. Ku, Yi-Chu Liu, Jer-Huei Lin
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引用次数: 1

摘要

采用薄层色谱法(TLC)、紫外光谱法(UV)、气相色谱-质谱法(GC-MS)和液相色谱-质谱法(LC-MS-MS)对中国大陆产中药胶囊中的枸橼酸西地那非(伟哥)和甲基睾酮进行了检测。采用高效液相色谱法对样品进行分析。在Inertsil ODS-2反相色谱柱上进行分离,以乙腈和0.1% (v/v)磷酸为流动相,梯度洗脱。以对羟基苯甲酸丙酯为内标,监测波长为254 nm。分别在80 ~ 800 μ/m L和20 ~ 200μ/m L范围内建立标准柠檬酸西地那非和甲基睾酮的校准曲线。枸橼酸西地那非和甲基睾酮在日间和日间的相对标准偏差分别为0.54- 3.56%和1.62- 3.75%。合成药物的回收率为98.0% ~ 100.4%。中草药中枸橼酸西地那非含量为20.0 mg/cap,甲基睾酮含量为1.6 mg/cap。
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High-performance Liquid Chromatographic Analysis of Sildenafil Citrate and Methyltestosterone Adulterants in a Herbal Medicine
Sildenafil citrate (Viagra) and methyltestosterone were detected in herbal medicine capsules from mainland China by thin layer chromatography (TLC), ultraviolet spectrometry (UV), gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass-mass spectrometry (LC-MS-MS). The sample was further assayed by high-performance liquid chromatography (HPLC). Separation was conducted on an Inertsil ODS-2 reversed-phase column using gradient: elution with acetonitrile and 0.1 % (v/v) phosphoric acid as the mobile phase. Propyl paraben was used as an internal standard and the monitor wavelength was 254 nm. Calibration curves of standard sildenafil citrate and methyltestosterone were constructed in the range of 80-800 and 20-200μ/m L, respectively. The relative standard deviations of sildenafil citrate and methyltestosterone for intra-day and inter-day analyses were 0.54-3.56 % and 1.62-3.75 %, respectively. The recoveries of the synthetic drugs from herbal medicine ranged from 98.0 to 100.4 %. The sildenafil citrate and methyltestosterone content in herbal medicine was 20.0 and 1.6 mg/cap, respectively.
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