Lu Yaling, Chen Jitao, Chen Bo, Yao Shouzhuo
Key Laboratory of Chemical Biology & Traditional Chinese Medicine Research, Ministry of Education, Hunan Normal University, Changsha 410081, China.
Se Pu. 2009 Jan;27(1):44-9.
A method of high performance liquid chromatography-mass spectrometry (HPLC-MS) for the simultaneous determination of 8 illegal synthetic drugs in antihypertensive dietary supplements was developed. The chromatography was performed using a Spherigel C18 column, with the mobile phase of 0.005 mol/L ammonium formate buffer (pH 3.0)-acetonitrile-methanol and cialis as internal standard. In ESI mode, the lowest concentration limit of detection (LOD) was 2.5 microg/L and the lowest concentration limit of quantification (LOQ) was 8.3 microg/L, while in ESI- mode, the lowest concentration limit of detection (LOD) was 50 microg/L. The average recoveries were between 63.3% - 107.4%. The clonidine, dihydrochlorothiazide, triamterene, metoprolol, phentolamine, chlorthalidone, furosemide and valsartan in the samples were separated well under the optimized conditions. The method was well validated by systematical searching for satisfactory conditions using the experimental designs including precision, repeatability and spiked recovery.
建立了一种高效液相色谱 - 质谱联用（HPLC - MS）法，用于同时测定抗高血压膳食补充剂中的8种非法合成药物。采用Spherigel C18柱进行色谱分析，流动相为0.005 mol/L甲酸铵缓冲液（pH 3.0） - 乙腈 - 甲醇，并以西地那非作为内标。在电喷雾电离（ESI）模式下，最低检测限（LOD）为2.5 μg/L，最低定量限（LOQ）为8.3 μg/L；而在负离子电喷雾电离（ESI -）模式下，最低检测限（LOD）为50 μg/L。平均回收率在63.3% - 107.4%之间。在优化条件下，样品中的可乐定、氢氯噻嗪、氨苯蝶啶、美托洛尔、酚妥拉明、氯噻酮、呋塞米和缬沙坦得到了很好的分离。该方法通过包括精密度、重复性和加标回收率在内的实验设计系统地寻找满意条件，得到了很好的验证。
