da Silva Danielle Cristina, Oliveira Cláudio Celestino
Universidade Tecnológica Federal do Paraná, Campus Dois Vizinhos, Estrada para Boa Esperança, Km 04 85660-000 Dois Vizinhos, PR, Brazil.
Departamento de Química, Universidade Estadual de Maringá, Avenida Colombo, 5790 87020-900 Maringá, PR, Brazil.
J Anal Methods Chem. 2018 Mar 1;2018:9143730. doi: 10.1155/2018/9143730. eCollection 2018.
Method for extraction and determination of amoxicillin, caffeine, ciprofloxacin, norfloxacin, tetracycline, diclofenac, ibuprofen, nimesulide, levonorgestrel, and 17-ethynylestradiol exploiting micellar liquid chromatography with PDA detector and solid-phase extraction was proposed. The usage of toxic solvents was low; the chromatographic separation of the medicaments was performed using a C18 column and mobile phases A and B containing 15.0% (v/v) ethanol, 3.0% (m/v) sodium dodecyl sulfate (SDS), and 0.02 mol·L phosphate at pHs 7.0 and 8.0, respectively. The method is simple, selective, and fast, and the analytes were separated in 23.0 min. For extraction, 1000 mL of sample containing 2.0% (v/v) ethanol and 0.002 mol·L citric acid at pH 2.50 was loaded through a 1000 mg of C18 cartridge. The analytes were eluted using 3.0 mL of ethanol, which were evaporated and redissolved in 0.5 mL of mobile phase. Concentration factors better than 1200, except amoxicillin (224), were obtained. The analytical curves were linear ( better than 0.992); LOD and LOQ (=10) presented values in the range of 0.019-0.247 and 0.058-0.752 mg·L, respectively. Recoveries of 99% were obtained, and the results are in agreement with those obtained by the comparative methods.
提出了一种利用带有光电二极管阵列检测器的胶束液相色谱法和固相萃取法提取并测定阿莫西林、咖啡因、环丙沙星、诺氟沙星、四环素、双氯芬酸、布洛芬、尼美舒利、左炔诺孕酮和炔雌醇的方法。有毒溶剂的用量很低；药物的色谱分离使用C18柱以及分别含有15.0%（v/v）乙醇、3.0%（m/v）十二烷基硫酸钠（SDS）和0.02 mol·L磷酸盐（pH分别为7.0和8.0）的流动相A和B进行。该方法简单、具有选择性且快速，分析物在23.0分钟内分离。对于萃取，将1000 mL含有2.0%（v/v）乙醇和0.002 mol·L柠檬酸（pH为2.50）的样品通过1000 mg的C18柱。使用3.0 mL乙醇洗脱分析物，将其蒸发并重新溶解于0.5 mL流动相中。除阿莫西林（224）外，获得了优于1200的浓缩因子。分析曲线呈线性（优于0.992）；检测限和定量限（=10）分别在0.019 - 0.247和0.058 - 0.752 mg·L范围内。回收率达到99%，结果与通过比较方法获得的结果一致。
