固相萃取分离-气相色谱-质谱法测定尿中18种邻苯二甲酸酯类增塑剂
GC-MS Determination of 18 Phthalates in Urine with Separation by Solid-Phase Extraction
摘 要
在尿样中加入混合同位素内标(D4-DBP和D4-DEHP)后,使之通过自制的SPE柱(取LC-C18填料,Envi-carb填料和PSA填料装入于玻璃柱中,用旋涡混合器使之混匀)对尿样中存在的邻苯二甲酯类化合物(PTA′s)进行SPE。SPE柱用正己烷-乙酸乙酯(1+1)混合液洗脱。用DB-5MS毛细管柱进行色谱分离,质谱分析中采用EI离子源和SIM模式进行测定,所测18种PTA′s在一定质量浓度范围内与峰面积呈线性关系,检出限(3S/N)在0.002 5~0.005 mg·kg-1之间。加标回收率在80.0%~120%之间,测定值的相对标准偏差(n=6)在2.5%~14%之间。
邻苯二甲酸酯类化合物
固相萃取
尿样
GC-MS
Phthalates
Solid-phase extraction
Urine samples
Abstract
Eighteen phthalates (PTA′s) in urine were separated on a self-made SPE column made by packing a glass column with fillers of LC-C18, Envi-carb and PSA and mixing with a swirling mixer. Mixed istopic PTA′s (i.e. D4-DBP and D4-DEHP) were added as internal standards. After passing the urine sample through the SPE column, the column was eluted with n-hexane-ethylacetate (1+1) mixture. DB-5MS capillary column was used for chromatographic separation, and EI as well as SIM mode was adopted in MS analysis. Linear relationships between values of peak area and mass concentration were obtained in definite ranges with values of DL (3S/N) ranged from 0.002 5 to 0.005 mg·kg-1. Values of recovery found by standard addition method were in the range of 80.0%-120%, with RSD′s (n=6) ranged from 2.5% to 14%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 国家自然科学基金(41101307);江苏省科技厅科技支撑计划项目(BE2010745);江苏省疾病预防控制中心“科教兴业工程”项目(JKRC2011030)资助
收稿日期 2013/5/22
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备注阮华(1988-),男,江苏盐城人,硕士研究生,研究方向为理化检验方法。
引用该论文: RUAN Hua,RONG Wei-guang,SONG Ning-hui,MA Yong-jian,JI Wen-liang,LIU Hua-liang. GC-MS Determination of 18 Phthalates in Urine with Separation by Solid-Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(7): 819～823
阮华,荣维广,宋宁慧,马永建,吉文亮,刘华良. 固相萃取分离-气相色谱-质谱法测定尿中18种邻苯二甲酸酯类增塑剂[J]. 理化检验－化学分册, 2014, 50(7): 819～823
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参考文献
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【3】YAN Hong-yuan, CHENG Xiao-ling, LIU Bao-mi. Simultaneous determination of six phthalate esters in bottled milks using ultrasound-assisted dispersive liquid-liquid microextraction coupled with gas chromatography［J］. Journal of Chromatography B, 2011,879(25):2507-2512.
【4】LUO Yan-bo, YU Qiong-wei, YUAN Bi-feng, et al. Fast microextraction of phthalate acid esters from beverage, environmental water and perfume samples by magnetic multi-walled carbon nanotubes［J］. Talanta, 2012,90:123-131.
【5】殷雪琰,许茜,吴淑燕,等.基于PA6纳米纤维膜固相萃取-液相色谱法检测牛奶中的邻苯二甲酸酯［J］.高等学校化学学报, 2010,31(4):690-695.
【6】RIOS J J, MORALES A, MRQUEZ-RUIZ G. Headspace solid-phase microextraction of oil matrices heated at high temperature and phthalate esters determination by gas chromatography multistage mass spectrometry［J］. Talanta, 2010,80(5):2076-2082.
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【8】ZHOU Xin, SHAO Xiao, SHU Jian-jun, et al. Thermally stable ionic liquid-based sol-gel coating for ultrasonic extraction-solid-phase microextraction-gas chromatography determination of phthalate esters in agricultural plastic films［J］. Talanta, 2012,89:129-135.
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【10】王成云,张绍文,张伟亚.PVC玩具和儿童用品中6种限用邻苯二甲酸酯类增塑剂的同时测定［J］.分析与测试, 2008(2):30-33.
【11】陈锦凤,易欢.β-环糊精修饰的金量子点对邻苯二甲酸酯类的检测［J］.武汉理工大学学报, 2011,33(6):107-110.
【12】GUO Liu, DONG Hui-ru. Trace determination of phthalate esters in river water by solvent sublation followed by high-performance liquid chromatography-ultraviolet detection［J］. International Journal of Environmental and Analytical Chemistry, 2009,89(5):357-365.
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【14】杨荣静,卫碧文,高欢,等.高效液相色谱-串联质谱法检测食品接触材料中的17种邻苯二甲酸酯类增塑剂［J］.环境化学, 2012,31(6):925-929.
【15】董静,潘玉香,朱莉萍,等.果蔬中54种农药残留的QuEChERS/GC-MS快速分析［J］.分析测试学报, 2008,27(1):66-69.
【16】MENKISSOGLU-SPIROUDI U, FOTOPOULOU A. Matrix effect in gas chromatographic determination of insecticides and fungicides in vegetables［J］. International Journal of Environmental Analytical Chemistry, 2004,84(1/3):15-27.
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