Manfio Josélia Larger, Santos Verônica Jorge, Lanchote Vera Lúcia, Santos Luciana M, Carmona Maria José C, Auler José Otavio Júnior, Brum Liberato Júnior, Donaduzzi Carmen Maria, Santos Silvia R C J
School of Pharmaceutical Sciences USP/SP, Av. Lineu Prestes, 580 Bloco 13a, Butantã-Cidade Universitária, CEP 05508-900, São Paulo-SP Brazil.
J AOAC Int. 2011 Jan-Feb;94(1):136-42.
A sensitive and fast HPLC/MS/MS method for measurement of sufentanil and morphine in plasma was developed and validated. A single liquid-liquid extraction in alkaline medium was used for the cleanup of plasma, and fentanyl was added as an internal standard (IS). The analyses were carried out using a C18 column and the mobile phase acetonitrile-5 mM ammonium acetate + 0.25% formic acid (70 + 30, v/v). The triple-quadrupole mass spectrometer equipped with an electrospray source in positive mode was set up in the selective reaction monitoring mode to detect precursor --> product ion transition 387.0 > 238.0, 285.7 > 165.1, and 337.0 > 188.0 for sufentanil, morphine, and IS, respectively. The method was linear in the 0.05 (LOQ) - 500 ng/mL range for sufentanil and 10 (LOQ) - 1000 ng/mL range for morphine. Good selectivity, linearity, precision, accuracy, and robustness were obtained for the HPLC/MS/MS method. The proposed method was successfully applied for the determination of sufentanil and morphine in patients undergoing cardiac surgery.
建立并验证了一种灵敏、快速的血浆中舒芬太尼和吗啡的高效液相色谱/串联质谱（HPLC/MS/MS）测定方法。采用在碱性介质中的单步液液萃取法对血浆进行净化，并加入芬太尼作为内标（IS）。分析使用C18柱，流动相为乙腈-5 mM醋酸铵+0.25%甲酸（70 + 30，v/v）。配备电喷雾源的三重四极杆质谱仪在正模式下以选择性反应监测模式运行，分别检测舒芬太尼、吗啡和内标的前体→产物离子跃迁387.0 > 238.0、285.7 > 165.1和337.0 > 188.0。该方法对舒芬太尼在0.05（定量下限）- 500 ng/mL范围内、对吗啡在10（定量下限）- 1000 ng/mL范围内呈线性。HPLC/MS/MS方法具有良好的选择性、线性、精密度、准确度和稳健性。所提出的方法成功应用于心脏手术患者中舒芬太尼和吗啡的测定。
