血清中盐酸曲马多的膜式固相萃取及GC/MS/SIM测定

Determination of Tramadol Hydrochloride in Serum Samples by Disk Solid Phase Extraction and Gas Chromatography-mass Spectrometry in Selected Ion Monitoring

目的建立血清中盐酸曲马多的膜式固相萃取(SPE)气-质联用分析方法。方法1mL血清用2mL0.1mol/L磷酸盐缓冲液(pH6)稀释后,用含有C18和强酸型强阳离子交换基团的SPECC18AR/MP3固相萃取柱萃取,洗脱液为含2%氨水的乙酸乙酯;选择SKF525作为内标物,用GC/MS/SIM定量测定。结果在加标量为0.1、0.2和0.5μg/mL的血清样品中,盐酸曲马多的回收率分别为98.9%、92.5%和84.8%,5次测定的RSD分别为3.2%、8.7%和10.9%;线性范围为0.1～4μg/mL,多项式回归相关系数r2=0.9939;检出限为21ng/mL;同一根萃取柱,连续使用5次,没有出现堵塞和污染,回收率及RSD未见下降。结论本方法适合于法医毒物分析。

Objective Disk solid phase extraction （SPE ）was assessed for tramadol hydrochloride from serum. Methods The SPE was performed with SPEC C18AR/MP3 Disk SPE cartridge, offering hydrophobic C18 and strong cation ionic exchange interactions for the analytes, before being added into extraction column, 1mL serum was diluted by 2 mL 0.1 mol/L phosphate buffer solution （pH 6） and the eluent was ethyl acetate containing 2% ammonia. Then SKF525 was added as internal standard into samples, which would be extracted simultaneously with analyte,quantitatively, determined by GC/MS/SIM. Results The extraction recovery of tramadol hydrochloride was 98.9%, 92.5% and 84.8% for serum samples with corresponding amounts of standard addition of 0.1 μg/mL, 0.2 μg/mL and 0.5 μg/mL. And RSD measured 5 times was 3.2%, 8.7% and 10.9% respectively. The linear range varied from 0.1 μg/mL to 4μg/mL. The multinomial regression correlation coefficient （r^2） equaled 0.9939, and the detection limit was 21 ng/mL. After the same extraction column was continuously used for 5 times, there was no jam, pollution and decline of recovery and RSD. Conclusion This method is suitable for forensic toxicological analysis.