A low solvent consumption method for the determination of non-steroidal anti-inflammatory drugs (NSAIDs) in animal urine samples is studied. The NSAIDs were extracted with CH2Cl2 by the ultrasound vortex assisted dispersive liquid–liquid microextraction (USVA-DLLME) method from urine samples, previously treated with β-glucuronidase/acrylsulfatase. After centrifugation, the bottom phase of the chlorinated solvent was separated from the liquid matrix, dried with Na2SO4, and derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) + trimethylchlorosilane (TMCS) (99 + 1). After cooling at room temperature, the solution was concentrated under nitrogen flow, and 1 µL of solution was analyzed in gas chromatography/ion trap-mass spectrometry (GC-IT-MS). The enrichment factor was about 300–450 times and recoveries ranged from 94.1 to 101.2% with a relative standard deviation (RSD) of ≤4.1%. The USVA-DLLME process efficiency was not influenced by the characteristics of the real urine matrix; therefore, the analytical method characteristics were evaluated in the range 1–100 ng mL−1 (R2 ≥ 0.9950). The limits of detection (LODs) and limits of quantification (LOQs) were between 0.1 and 0.2 ng mL−1 with RSD ≤4.5% and between 4.1 and 4.7 ng mL−1 with RSD ≤3.5%, respectively, whereas inter- and intra-day precision was 3.8% and 4.5%, respectively. The proposed analytical method is reproducible, sensitive, and simple.

中文翻译：

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超声涡流辅助分散液-液微萃取和气相色谱联用离子阱质谱法测定动物尿液样品中的非甾体抗炎药

研究了一种用于测定动物尿样中非甾体抗炎药 (NSAID) 的低溶剂消耗方法。NSAIDs 用 CH2Cl2 通过超声涡流辅助分散液-液微萃取 (USVA-DLLME) 方法从尿样中提取，之前用 β-葡萄糖醛酸酶/丙烯酰硫酸酯酶处理过。离心后，将氯化溶剂的底部相与液体基质分离，用 Na2SO4 干燥，并用 N,O-双（三甲基甲硅烷基）三氟乙酰胺 (BSTFA) + 三甲基氯硅烷 (TMCS) (99 + 1) 衍生化。室温冷却后，溶液在氮气流下浓缩，1 µL 溶液用气相色谱/离子阱质谱 (GC-IT-MS) 分析。富集因子约为 300-450 倍，回收率范围为 94.1 至 101。2%，相对标准偏差 (RSD) ≤ 4.1%。USVA-DLLME 处理效率不受真实尿液基质特性的影响；因此，在 1–100 ng mL-1 (R2 ≥ 0.9950) 范围内评估了分析方法特性。检测限 (LOD) 和定量限 (LOQ) 分别在 0.1 和 0.2 ng mL-1 之间，RSD ≤ 4.5% 和 4.1 和 4.7 ng mL-1 之间，RSD ≤ 3.5%，而-day 精度分别为 3.8% 和 4.5%。所提出的分析方法具有重现性、灵敏性和简单性。检测限 (LOD) 和定量限 (LOQ) 分别在 0.1 和 0.2 ng mL-1 之间，RSD ≤ 4.5% 和 4.1 和 4.7 ng mL-1 之间，RSD ≤ 3.5%，而-day 精度分别为 3.8% 和 4.5%。所提出的分析方法具有重现性、灵敏性和简单性。检测限 (LOD) 和定量限 (LOQ) 分别在 0.1 和 0.2 ng mL-1 之间，RSD ≤ 4.5% 和 4.1 和 4.7 ng mL-1 之间，RSD ≤ 3.5%，而-day 精度分别为 3.8% 和 4.5%。所提出的分析方法具有重现性、灵敏性和简单性。