HPLC Determination of 2 Metabolites of Monochlorobenzene in Urine with Surfactant Assisted Microextraction
摘 要
尿样以十六烷基三甲基溴化铵为辅助剂,正辛醇为萃取剂,萃取液离心后,取上层有机相,采用高效液相色谱法测定其中一氯苯的2种代谢物(4-氯邻苯二酚和对氯苯酚)的含量。以RD-C18色谱柱为分离柱,以甲醇与0.15%(体积分数)的磷酸溶液以体积比65:35组成的混合液为流动相,在检测波长280 nm处进行测定。4-氯邻苯二酚和对氯苯酚的质量浓度均在600 μg·L-1以内与其对应的峰面积呈线性关系,检出限(3S/N)为1.67,2.23 μg·L-1,测定下限(10S/N)为5.55,7.43 μg·L-1。以空白样品为基体进行加标回收试验,所得回收率为89.2%~97.4%,测定值的日内相对标准偏差(n=6)为2.1%~4.9%,日间相对标准偏差(n=18)为2.5%~5.3%。
Abstract
The urine sample was extracted with n-octanol with hexadecyl trimethyl ammonium bromide as auxiliary solvent. The extract was centrifugated, and then the upper organic phase was taken. HPLC was applied to the determination of 2 metabolites (4-chlorocatechol and p-chlorophenol) of monochlorobenzene in the upper organic phase. RD-C18 chromatographic column was used as separation column, and a mixture of methanol and 0.15% (φ) phosphoric acid solution with volume ratio of 65∶35 was used as mobile phase. Detection at 280 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of 4-chlorocatechol and p-chlorophenol were kept in the same range within 600 μg·L-1, with detection limits (3S/N) of 1.67, 2.23 μg·L-1 and lower limits of determination (10S/N) of 5.55, 7.43 μg·L-1 respectively. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 89.2%-97.4%, with intra-day RSDs (n=6) and inter-day RSDs (n=18) of determined values in the ranges of 2.1%-4.9%, 2.5%-5.3%, respectively.
中图分类号 O652.63 DOI 10.11973/lhjy-hx202005004
所属栏目 工作简报
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收稿日期 2019/10/9
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备注盛旭光,硕士研究生,研究方向为卫生检验与检疫
引用该论文: SHENG Xuguang,MEI Yong,NIE Menghan,CHEN Haichuan,WANG Gang. HPLC Determination of 2 Metabolites of Monochlorobenzene in Urine with Surfactant Assisted Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(5): 519~524
盛旭光,梅勇,聂梦涵,陈海川,王港. 表面活性剂辅助微萃取-高效液相色谱法测定尿中一氯苯的2种代谢物[J]. 理化检验-化学分册, 2020, 56(5): 519~524
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【3】朱杰,罗启仕,郭琳,等.碱热活化过硫酸盐氧化水中氯苯的试验[J].环境化学, 2013,32(12):2256-2262.
【4】PANDELOVA M, LENOIR D, SCHRAMM K W. Correlation between PCDD/F, PCB and PCBz in coal/waste combustion.Influence of various inhibitors[J]. Chemosphere, 2006,62(7):1196-1205.
【5】HE Y, WANG Y, LEE H K. Trace analysis of ten chlorinated benzenes in water by headspace solid-phase microextraction[J]. Journal of Chromatography A, 2000,874(1):149-154.
【6】MEHARG A, WRIGHT J, OSBORN D. Chlorobenzenes in rivers draining industrial catchments[J]. Science of the Total Environment, 2000,251/252:243-253.
【7】KNECHT U, WOITOWITZ H J. Human toxicokinetics of inhaled monochlorobenzene:Latest experimental findings regarding re-evaluation of the biological tolerance value[J]. International Archives of Occupational and Environmental Health, 2000,73(8):543-554.
【8】REZAEE M, YAMINI Y, FARAJI M. Evolution of dispersive liquid-liquid microextraction method[J]. Journal of Chromatography A, 2010,1217(16):2342-2357.
【9】WANG Q F, CHEN R J, SHATNER W, et al. State-of-the-art on the technique of dispersive liquid-liquid microextraction[J]. Ultrasonics Sonochemistry, 2019,51:369-377.
【10】FERRONE V, COTELLESE R, CARLUCCI M, et al. Air assisted dispersive liquid-liquid microextraction with solidification of the floating organic droplets (AA-DLLME-SFO) and UHPLC-PDA method:Application to antibiotics analysis in human plasma of hospital acquired pneumonia patients[J]. Journal of Pharmaceutical and Biomedical Analysis, 2018,151:266-273.
【11】SARAJI M, BIDGOLI A A H. Dispersive liquid-liquid microextraction using a surfactant as disperser agent[J]. Analytical and Bioanalytical Chemistry, 2010,397(7):3107-3115.
【12】SPIETELUN A, MARCINKOWSKI Ł, DE LA GUARDIA M, et al. Green aspects,developments and perspectives of liquid phase microextraction techniques[J]. Talanta, 2014,119:34-45.
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【14】MORADI M, YAMINI Y, ESRAFILI A, et al. Application of surfactant assisted dispersive liquid-liquid microextraction for sample preparation of chlorophenols in water samples[J]. Talanta, 2010,82(5):1864-1869.
【15】BEHBAHANI M, NAJAFI F, BAGHERI S, et al. Application of surfactant assisted dispersive liquid-liquid microextraction as an efficient sample treatment technique for preconcentration and trace detection of zonisamide and carbamazepine in urine and plasma samples[J]. Journal of Chromatography A, 2013,1308:25-31.
【16】EBRAHIMPOUR B, YAMINI Y, MORADI M. Application of ionic surfactant as a carrier and emulsifier agent for the microextraction of fluoroquinolones[J]. Journal of Pharmaceutical and Biomedical Analysis, 2012,66:264-270.
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