~1H qNMR检测保健食品中抗疲劳西药成分的方法研究
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- 英文论文题名：Determination of Anti-fatigue Pharmaceutical Components in Dietary Supplements by ~1H qNMR
- 论文作者：张志强 ; 王丽娟 ; 涂光忠 ; 安东各 ; 赵阳
- 英文论文作者：Zhang Zhiqiang ; Wang Lijuan ; Tu Guangzhong ; An Dongge ; Zhao Yang ; Beijing Institute of Microchemistry ; Institut of Forensic Science ; Ministry of Public Security P.R.C
- 年：2016
- 作者机构：北京微量化学研究所;公安部物证鉴定中心;
- 论文关键词：定量核磁共振 ; 保健食品 ; 枸橼酸西地那非 ; 他达拉非 ; 伐地那非
- 英文论文关键词：qNMR ; Dietary Supplements ; Sildenafil citrate ; Tadalafil ; Vardenafil
- 会议召开时间：2016-07-01
- 会议录名称：中国化学会第30届学术年会摘要集-第三十四分会：公共安全化学
- 语种：中文
- 分类号：O657.2;TS218
- 学会代码：ZGHY
- 会议名称：中国化学会第30届学术年会-第三十四分会 ; 公共安全化学
- 会议地点：中国辽宁大连
- 主办单位：中国化学会
- 学会名称：中国化学会
- 页数：1
- 文件大小：188k
- 原文格式：D
- 会议级别：全国
摘要
本文建立了保健食品中非法添加枸橼酸西地那非、他达拉非、伐地那非等西药成分的核磁共振氢谱定量方法(~1H qNMR),并进行了方法学验证。实验采用布鲁克Avance DRX 500超导核磁共振波谱仪,以氘代二甲亚砜为溶剂,2,3,5-三碘苯甲酸为内标物;实验对检测参数进行了优化:谱宽8012Hz,中心频率3250Hz,脉冲宽度8μs,弛豫延迟时间20秒,扫描次数最低8次。方法验证结果表明,内标添加量为2mg时,该方法检测枸橼酸西地那非、他达拉非和伐地那非的线性方程相关系数R2≥0.999,线性良好;3种化合物的最低检出限分别为:0.046mg/m L、0.023mg/m L、0.030mg/m L,定量限分别为0.197mg/m L、0.114mg/mL、0.152mg/m L;该方法日内精密度RSD值分别为:0.38%、0.85%、0.34%,日间精密度RSD值分别为:0.72%、1.25%、1.36%。实验通过与HPLC-DAD法测试相同样品,验证了~1H qNMR法的准确性。试验结果表明两种方法的测定结果 RSD值在1%~8%之间。
In this thesis, a method of ~1H qNMR was developed, for the determination of Sildenafil Citrate, Tadalafil, Vardenafil added in dietary supplements illegally. In this experiments, Bruker Avance DRX 500 was applied, with DMSO-d6 as solvent and 2,3,5-Triiodobenzoic acid as internal standard substance, the spectral width is set to 8012 Hz, the center frequency is set to 3250 Hz, the pulse width is set to 8μs, relaxation delay time is set to 20 seconds, the number of scans is set to a minimum of 8 times. The correlation coefficient from the linear regression was higher than 0.999. The lowest detection limit of the method for sildenafil citrate, tadalafil and vardenafil were 0.046 mg/mL 、0.023 mg/mL 、0.030 mg/mL, and the low limit of quantitation were 0.197 mg/mL 、0.114 mg/mL 、0.152 mg/mL. RSD values of within-day precision were as follows: 0.38%, 0.85%, 0.34%, day to day precision RSD values were as follows: 0.72%, 1.25%, 1.36%.The accuracy of the method was also verified by comparing the results of ~1H qNMR and HPLC-DAD, testing the same samples. The results showed that the RSD values of the two methods were around 1%~8%.
In this thesis, a method of ~1H qNMR was developed, for the determination of Sildenafil Citrate, Tadalafil, Vardenafil added in dietary supplements illegally. In this experiments, Bruker Avance DRX 500 was applied, with DMSO-d6 as solvent and 2,3,5-Triiodobenzoic acid as internal standard substance, the spectral width is set to 8012 Hz, the center frequency is set to 3250 Hz, the pulse width is set to 8μs, relaxation delay time is set to 20 seconds, the number of scans is set to a minimum of 8 times. The correlation coefficient from the linear regression was higher than 0.999. The lowest detection limit of the method for sildenafil citrate, tadalafil and vardenafil were 0.046 mg/mL 、0.023 mg/mL 、0.030 mg/mL, and the low limit of quantitation were 0.197 mg/mL 、0.114 mg/mL 、0.152 mg/mL. RSD values of within-day precision were as follows: 0.38%, 0.85%, 0.34%, day to day precision RSD values were as follows: 0.72%, 1.25%, 1.36%.The accuracy of the method was also verified by comparing the results of ~1H qNMR and HPLC-DAD, testing the same samples. The results showed that the RSD values of the two methods were around 1%~8%.
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