Iqbal Muzaffar, Ezzeldin Essam, Haq Nazrul, Alam Prawez
Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, Riyadh 11451, Saudi Arabia.
Bioavailability Unit, Central Laboratory, College of Pharmacy, King Saud University, Riyadh 11451, Saudi Arabia.
ACS Omega. 2021 Mar 10;6(11):7524-7532. doi: 10.1021/acsomega.0c06047. eCollection 2021 Mar 23.
A novel, simple, and reliable ultraperformance liquid chromatography tandem-mass spectrometry (UPLC-MS/MS ) assay based on dispersive liquid-liquid microextraction followed by ultrasound-assisted reverse extraction from solidified floating organic droplets was established for determination of multiclass pharmaceuticals in the water sample. Six commonly used drugs of various therapeutic classes: ibuprofen, ketorolac, lamotrigine, propranolol, pantoprazole, and losartan were extracted from water samples by using 50 μL 1-undecanol as extracting solvent and 400 μL acetonitrile as dispersive solvent. After collecting the floating organic droplets by cold centrifugation, an ultrasound-assisted back extraction procedure was performed to make the sample compatible for UPLC-MS/MS analysis. Acquity BEH C column (2.1 × 100; 1.7 μm) was used for separation of target analytes that were eluted by a gradient mobile phase composition of 15 mM ammonium acetate and acetonitrile at a flow rate of 0.25 mL/min. The sample ionization was performed by using electrospray ionization in positive mode, and multiple reaction monitoring was used for quantification of target analytes. After optimizing the assay conditions, all calibration curves were found to be linear with limit of detection and limit of quantification were ranged in between 0.06-0.15 and 0.16-0.41 ng/mL, respectively. The enrichment factor was found to be 172-192-fold and the relative recovery was ranged between 93.1 and 109.4% between target analytes. These satisfactory results confirmed that the proposed method is specific and reliable for application of trace analysis of target analytes in waste water samples.
建立了一种基于分散液液微萃取，随后从固化漂浮有机液滴中进行超声辅助反萃取的新型、简单且可靠的超高效液相色谱串联质谱（UPLC-MS/MS）分析方法，用于测定水样中的多类药物。使用50 μL 1-十一醇作为萃取溶剂、400 μL乙腈作为分散溶剂，从水样中萃取六种不同治疗类别的常用药物：布洛芬、酮咯酸、拉莫三嗪、普萘洛尔、泮托拉唑和氯沙坦。通过冷离心收集漂浮有机液滴后，进行超声辅助反萃取程序，使样品适合UPLC-MS/MS分析。采用Acquity BEH C柱（2.1×100；1.7 μm）分离目标分析物，以15 mM醋酸铵和乙腈的梯度流动相组成在0.25 mL/min的流速下进行洗脱。采用正模式电喷雾电离进行样品电离，并使用多反应监测对目标分析物进行定量。优化分析条件后，所有校准曲线均呈线性，检测限和定量限分别在0.06 - 0.15和0.16 - 0.41 ng/mL之间。富集因子为172 - 192倍，目标分析物之间的相对回收率在93.1%至109.4%之间。这些令人满意的结果证实了所提出的方法对于废水样品中目标分析物的痕量分析应用具有特异性和可靠性。
