微柱萃取与高效液相色谱联用测定镇定剂残留
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摘要
环境水和血液样品中镇静剂残留浓度低,且基质复杂,干扰严重,需经高效样品前处理技术对目标物进行富集分离。采用C_(18)微柱离心萃取解吸的新型微萃取模式,与高效液相色谱联用,建立了环境水和血样中三唑仑、安定和唑吡坦3种镇静剂残留的分析方法。研究结果表明,NaCl浓度为0.35 g/mL条件下萃取效果最佳。在最佳条件下,3种镇定剂在20～200μg/L范围内与峰面积呈良好的线性关系,相关系数均大于0.99。三唑仑、安定和唑吡坦的检出限分别为2.51μg/L,2.67μg/L和3.36μg/L。用于河水和血液样品中镇定剂残留测定,平均加标回收率高于84%。
Due to low trace mount of sedative residues and the complicated matrix of environmental water and blood, it is necessary to develop an efficient sample pretreatment process for the enrichment and separation of target analytes prior to analysis. A new solid phase microextraction model based on the combination between C_(18) micropillar and high performance liquid chromatography(HPLC) is used for the determination of triazolam, diazepam and zolpidem in environmental water and blood samples. The experimental result shows that the best extraction efficiency is obtained under 0.35 g/mL NaCl. Under the optimum condition, the linear range of the three sedatives is 20～200 μg/L, with the correlation coefficients(R~2) greater than 0.99. The detection limits of triazolam, diazepam and zolpidem are 2.51 μg/L, 2.67 μg/L and 3.36 μg/L respectively. The method is applied for the determination of sedative residues in river water and blood samples, and the average recovery rates are higher than 84%.
Due to low trace mount of sedative residues and the complicated matrix of environmental water and blood, it is necessary to develop an efficient sample pretreatment process for the enrichment and separation of target analytes prior to analysis. A new solid phase microextraction model based on the combination between C_(18) micropillar and high performance liquid chromatography(HPLC) is used for the determination of triazolam, diazepam and zolpidem in environmental water and blood samples. The experimental result shows that the best extraction efficiency is obtained under 0.35 g/mL NaCl. Under the optimum condition, the linear range of the three sedatives is 20～200 μg/L, with the correlation coefficients(R~2) greater than 0.99. The detection limits of triazolam, diazepam and zolpidem are 2.51 μg/L, 2.67 μg/L and 3.36 μg/L respectively. The method is applied for the determination of sedative residues in river water and blood samples, and the average recovery rates are higher than 84%.
引文
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[3] 郭鹏,宿娜,许晓宇,等.固相萃取人体血液中安定条件的统计学筛选与相应面优化[J].分析实验室,2012,31(8):36-39.
[4] 魏欣,安静,吴茵,等.UPLC-MS/MS法同时检测人血浆中唑吡坦、右佐匹克隆和扎来普隆的方法研究[J].中国药房,2016,27(23):3194-3197.
[5] DE BOECK M,DAMILANO G,DEHAEN W,et al.Evaluation of 11 ionic liquids as potential extraction solvents for benzodiazepines from whole blood using liquid-liquid microextraction combined with LC-MS/MS[J].Talanta,2018,184:369-374.
[6] MENG L,ZHU B L,ZHENG K F,et al.Ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction for the determination of 4 designer benzodiazepines in urine samples by gas chromatography-triple quadrupole mass spectrometry[J].Journal of Chromatography B,2017,1053:9-15.
[7] 甘蓓,况慧娟,涂瑾.磁固相萃取-液相色谱-串联质谱法检测牛肉中4种苯二氮卓类药物的残留[J].食品安全质量检测学报,2015,6(9):3677-3683.
[8] ZHANG S L,YAO W X,FU D F,et al.Fabrication of magnetic zinc adeninate metal-organic frameworks for the extraction of benzodiazepines from urine and wastewater[J].Journal of Separation Science,2018,41(8):1864-1870.
[9] YAO W,FAN Z,ZHANG S,et al.Poly(methacrylic acid-ethylene glycol dimethacrylate-N-vinylcarbazole) monolithic column for the enrichment of trace benzodiazepines from urine and beer samples[J].Journal of Separation Science,2017,40(6):1369-1376.
[10] YAO W X,FAN Z F,ZHANG S L,et al.Graphene-modified monolithic capillary column for the microextraction of trace benzodiazepines in biological samples[J].Analytical Letters,2017,50(18):2869-2883.