Omotola Elizabeth Oyinkansola, Olatunji Olatunde Stephen
School of Chemistry and Physics, University of KwaZulu-Natal, Westville, Durban 4000, South Africa.
Department of Chemistry, Tai Solarin University of Education, Ijebu Ode, Ogun State, Nigeria.
Heliyon. 2020 Dec 28;6(12):e05787. doi: 10.1016/j.heliyon.2020.e05787. eCollection 2020 Dec.
The detection and quantitation of pharmaceutical compounds (PCs) in different environmental matrices is still a challenge, due to their extremely low (ng-μg) concentrations and the lack of rapid and sensitive analytical techniques. A number of techniques, such as enzyme-linked immunosorbent assay (ELISA), chromatography, electrophoresis, and electrochemical methods have been explored. These methods are limited by their poor sensitivity. In this study, a hyphenated liquid chromatography-mass spectrometric (LC-MS) method was developed, validated, and tested for the detection and quantification of seven active pharmaceutical compounds, with solid-phase extraction for analytes recovery and separation of interference from the aqueous matrix. The sensitivity achieved for the method allowed for LODs (μg/L) of 0.0439, 0.0684, 0.1219, 0.0710, 0.1129, 0.0447, 0.0837 and LOQs (μg/L) of 0.1462, 0.2281, 0.4065, 0.2367, 0.3763, 0.1492, 0.2792, for lamivudine, acetaminophen, vancomycin, ciprofloxacin, sulfamethoxazole, diclofenac, and ivermectin, respectively, within a linear range of 0.01-0.1 μg/mL. Other ICH validation parameters are also discussed. The different PCs were positive in 61 % of the tested surface waters, with diclofenac present only in two of the sampling points. The concentrations at which they occurred were variable and ranged between ND and 398.98 μg/L.
由于药物化合物(PCs)在不同环境基质中的浓度极低(纳克至微克级),且缺乏快速灵敏的分析技术,因此对其进行检测和定量分析仍然是一项挑战。人们已经探索了多种技术,如酶联免疫吸附测定法(ELISA)、色谱法、电泳法和电化学方法。但这些方法的灵敏度较低。在本研究中,开发并验证了一种联用液相色谱 - 质谱(LC - MS)的方法,用于检测和定量七种活性药物化合物,采用固相萃取法回收分析物并分离水基质中的干扰物。该方法的灵敏度使得拉米夫定、对乙酰氨基酚、万古霉素、环丙沙星、磺胺甲恶唑、双氯芬酸和伊维菌素的检测限(μg/L)分别为0.0439、0.0684、0.1219、0.0710、0.1129、0.0447、0.0837;定量限(μg/L)分别为0.1462、0.2281、0.4065、0.2367、0.3763、0.1492、0.2792,线性范围为0.01 - 0.1μg/mL。还讨论了其他国际协调会议(ICH)验证参数。在所测试的地表水样本中,61%检测出不同的PCs呈阳性,其中双氯芬酸仅在两个采样点被检测到。它们出现的浓度各不相同,范围在未检出(ND)至398.98μg/L之间。