Rajasekhar Damaramadugu, Kumara Inamadugu Jaswanth, Venkateswarlu Ponneri
Analytical and Environmental Chemistry Division, Department of Chemistry, Sri Venkateswara University, Tirupati 517 502, India.
Eur J Mass Spectrom (Chichester). 2009;15(6):715-21. doi: 10.1255/ejms.1038.
A sensitive, selective and rapid liquid chromatography/tandem mass spectrometric (LC-MS/MS) method was developed and validated for the determination of hydrochlorothiazide (HCTZ) in human plasma. The plasma samples were prepared by solid phase extraction using Oasis HLB 30 mg 1CC cartridges. Chromatographic separation was accomplished on a Thermo Hypurity Advance (50 mm x 4.6mm i.d., 5 microm) column. The mobile phase consisted of HPLC Grade Acetonitrile: 2 mM Ammonium acetate (90 : 10 v / v) at a flow rate of 0.5 mL min(-1). Detection of hydrochlorothiazide and the internal standard (IS) zidovudine was achieved by ESI MS/MS in the negative ion mode. The total chromatographic runtime was 2.5 minutes. The linear range of the method was from 2.036-203.621 ng mL(-1). The mass transition ion pair has been followed as m/z 296.10/205.00 for HCTZ and 266.10/223.10 for Zidovudine. The mean overall recovery of HCTZ was 66.40% with a precision of 2.44%. The mean recovery of internal standard (Zidovudine) was 63.62% with a precision ranging from 2.06% to 5.40%. The method was successfully applied for the evaluation of pharmacokinetics of hydrochlorothiazide after single oral dose of 25 mg hydrochlorothiazide to healthy volunteers.
建立了一种灵敏、选择性好且快速的液相色谱/串联质谱（LC-MS/MS）法，并对其进行了验证，用于测定人血浆中的氢氯噻嗪（HCTZ）。血浆样品采用Oasis HLB 30 mg 1CC柱进行固相萃取制备。色谱分离在Thermo Hypurity Advance柱（50 mm×4.6mm内径，5μm）上完成。流动相由HPLC级乙腈：2 mM醋酸铵（90:10 v/v）组成，流速为0.5 mL min(-1)。氢氯噻嗪和内标（IS）齐多夫定通过电喷雾电离串联质谱（ESI MS/MS）在负离子模式下进行检测。总色谱运行时间为2.5分钟。该方法的线性范围为2.036 - 203.621 ng mL(-1)。HCTZ的质量转移离子对为m/z 296.10/205.00，齐多夫定的质量转移离子对为m/z 266.10/223.10。HCTZ的平均总回收率为66.40%，精密度为2.44%。内标（齐多夫定）的平均回收率为63.62%，精密度范围为2.06%至5.40%。该方法成功应用于对25 mg氢氯噻嗪单次口服给药健康志愿者后氢氯噻嗪的药代动力学评价。
