School of Chemistry and Physics, University of KwaZulu-Natal, Private Bag X 54001, Durban, 4000, South Africa.
Department of Chemistry, Mbarara University of Science and Technology, Private Bag, 1410, Mbarara, Uganda.
Environ Sci Pollut Res Int. 2017 Aug;24(24):20015-20028. doi: 10.1007/s11356-017-9653-6. Epub 2017 Jul 11.
The occurrence of eight pharmaceuticals was monitored during four seasons (spring, summer, autumn, and winter) along a 250-km stretch of the Msunduzi and Mgeni rivers in KwaZulu-Natal, South Africa. This paper describes an optimized method for the determination of nonsteroidal anti-inflammatory drugs (NSAIDs) in sediments. The method combines ultrasonic, centrifuge, and gas chromatography-mass spectrometry for the detection of these drugs in solid samples. Most of the parameters that affect the extraction step were optimized. Solid samples were placed in a centrifuge tube and extracted with ethyl acetate:acetone (1:1, two cycles), followed by clean-up with Oasis HLB cartridge and derivatization with N, O-bis(trimethylsilyl) trifluoroacetamide (BSTFA). Satisfactory recoveries were obtained ranging from 66 to 130%, depending on the analyte. Precision expressed as RSD (%) (n = 3) was less than 20% for all analytes. The LODs and LOQs were in the range of 0.024 to 1.90 ng g which allowed to be applied in the analysis solid samples in Msunduzi and Mgeni rivers. In the solid samples analyzed, NSAID concentration ranged from not detected to 221 ng g.
本研究沿南非夸祖鲁-纳塔尔省的姆森祖鲁河和姆根尼河 250 公里河段,在四季(春季、夏季、秋季和冬季)监测了 8 种药物的存在情况。本文描述了一种优化的方法,用于测定沉积物中的非甾体抗炎药(NSAIDs)。该方法结合了超声波、离心和气相色谱-质谱法,用于检测这些药物在固体样品中的存在。优化了影响提取步骤的大多数参数。将固体样品置于离心管中,用乙酸乙酯:丙酮(1:1,两个循环)提取,然后用 Oasis HLB 小柱进行净化,并用 N, O-双(三甲基硅基)三氟乙酰胺(BSTFA)衍生化。根据分析物的不同,回收率在 66%至 130%之间,令人满意。所有分析物的精密度(RSD,%)(n=3)均小于 20%。LOD 和 LOQ 范围在 0.024 至 1.90ng g 之间,允许应用于姆森祖鲁河和姆根尼河的固体样品分析。在所分析的固体样品中,NSAID 浓度范围从未检出到 221ng g。