Determination of steroid sex hormones in real matrices by bar adsorptive microextraction (BAμE).

摘要: In the present work, development of a novel analytical approach which combines miniaturized bar adsorptive microextraction device with micro-liquid desorption in one single step, followed by high performance liquid chromatography diode array detection (BAµE-µLD/HPLC–DAD), is proposed for determination trace levels nine steroid hormones (estriol, 17s-estradiol, 17α-estradiol, 19-northisterone, 17α-ethynylestradiol, estrone, d-(-)-norgestrel, progesterone and mestranol) environmental biological matrices. From comparison ten different coating phases (five polymeric five activated carbon sorbents), modified pyrrolidone polymer (P2) showed best compromise between selectivity efficiency. Assays performed through BAµE(P2, 1.3 mg)-µLD(100 µL)/HPLC–DAD on 25 mL ultrapure water samples spiked at 6.0 μg/L level, yielded recoveries ranging from 93±9% to 101±8%, under optimized experimental conditions. The convenient (50.0–100.0 ng/L) quantification limits (165.0–330.0 ng/L), as well good linear dynamic ranges (0.2–24.0 µg/L) remarkable coefficients (r2>0.9968). Excellent repeatability were also achieved intraday (RSD<14%) interday (RSD<12%) experiments. application urine samples, using standard addition methodology (SAM), revealed linearity sensitivity some target compounds. short, miniaturization combined minimization solvent volume back-extraction step demonstrated performance, increasing enrichment factor, being simultaneously more easier implement environment friendly.