HPLC Determination of 6 Phthalates in Soil and Evaluation of Its Biological Availability
摘 要
取土壤样品10.000 g两份,其中一份用10 mL甲醇超声提取30 min使其所含6种邻苯二甲酸酯(PAEs)[包括邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁基苄酯(BBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基)己酯(DEHP)及邻苯二甲酸二辛酯(DNOP)]溶于甲醇中。于提取液中加入硫酸镁和氯化钠,离心3 min。取上清液,定容至10.0 mL。经0.45 μm滤膜过滤,取滤液按色谱条件进行测定。以Zorbax Eclipse C18色谱柱为固定相,以不同比例的乙腈(A)和水(B)的混合液为流动相进行梯度洗脱,并用紫外检测器于245 nm处测定。上述6种PAEs的质量浓度均在0.10~10.0 mg·L-1内与其对应的色谱峰面积呈线性关系,检出限在0.01~0.04 mg·L-1之间。另一份样品先用10 mL胃液在37℃振荡提取1 h,用碳酸氢钠调节消化液pH至7.0,加入55.0 mg胆汁盐和15 mg胰液素,在37℃振荡提取2 h,完成体外胃肠模拟处理。经离心3 min,取上清液,按上述方法加入甲醇提取,并用高效液相色谱法进行测定。所得结果表明:PAEs的脂溶性越高,其生物有效性越低。此外,土壤的理化参数对PAEs的生物有效性也有影响。
Abstract
Two portions (10.000 g. each) of the soil sample were taken, and one portion (10 mL) of methanol were added to extract the 6 phthalates[i.e., dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl benzyl phthalate (BBP), dibutyl phthalate (DBP), di-(2-ethyl)hexylphthalate (DEHP) and dioctylphthalate (DNOP)], into the methanol phase with the aid of ultrasonotor for 30 min. Appropriate amounts of MgSO4 and NaCl were added to the extract, and the mixture was centrifuged for 3 min. The supernatant was diluted to 10.0 mL and filtered through 0.45 μm filtering membrane. The filtrate was analyzed by HPLC. Zorbax Eclipse C18 chromatographic column was used as stationary phase. Mixtures of acetonitrile (A) and water (B) with various ratios were used as mobile phase in the programmed gradient elution. And the 6 phthalates were determined by UV-detector at 245 nm. Linear relationships between values of chromatographic peak areas and corresponding mass concentrations of the 6 phthalates were found in the same range of 0.10-10.0 mg·L-1. Detection limits found were in the range of 0.01-0.04 mg·L-1. Another portion of the sample was treated by invitro gastrointestinal simulation with successive extractions in the following way:The sample was first extracted with 10 mL of the simulated gastric juice for 1 h at 37℃, to obtain the digestive juice, which, after adjusting its pH to 7.0 with NaHCO3, and addition of 55.0 mg of bile salt and 15 mg of pancreatic secretin (acting as simulated intestinal juice) was extracted by vibration for 2 h at 37℃. After centrifuging for 3 min, the supernatant was taken and treated by the procedure given above beginning from extraction with methanol. It was found that the biological availability of the PAEs tended to giver lower rates as their fat-solubility are higher. In addition, the biological availability of the PAEs was also effected by physical and chemical properties of the soil.
中图分类号 O652.63 DOI 10.11973/lhjy-hx202002015
所属栏目 工作简报
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收稿日期 2019/4/27
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备注刘成霞,工程师,硕士研究生,主要从事化学分析与检测方法研究工作
引用该论文: LIU Chengxia,ZHU Yang,LIU Lüye. HPLC Determination of 6 Phthalates in Soil and Evaluation of Its Biological Availability[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(2): 206~210
刘成霞,朱洋,刘绿叶. 高效液相色谱法测定土壤中6种邻苯二甲酸酯的含量及其生物有效性的评价[J]. 理化检验-化学分册, 2020, 56(2): 206~210
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参考文献
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【3】曹莹,陈莎,王晓伟,等.环境中邻苯二甲酸酯类化合物的分析测定[J].环境与健康杂志, 2007,24(7):546-549.
【4】SUN J, WU X, GAN J. Uptake and metabolism of phthalate esters by edible plants[J]. Environmental Science & Technology, 2015,49(14):8471-8478.
【5】BUI T T, ALVES A, PALM-COUSINS A, et al. Estimating uptake of phthalate ester metabolites into the human nail plate using pharmacokinetic modelling[J]. Environment International, 2017,100:148-155.
【6】WINE R N, LI L H, BARNES L H, et al. Reproductive toxicity of di-n-butylphthalate in a continuous breeding protocol in Sprague-Dawley rats[J]. Environmental Health Perspectives, 1997,105(1):102-107.
【7】卢佑演,湛社霞,孙世宏,等.HPLC法测定饮料中6种邻苯二甲酸酯类塑化剂的研究[J].中国卫生检验杂志, 2013,23(11):2410-2412.
【8】STAPLES C A, GUINN R, KRAMARZ K, et al. Assessing the chronic aquatic toxicity of phthalate ester plasticizers[J]. Human and Ecological Risk Assessment:an International Journal, 2011,17(5):1057-1076.
【9】李韵姿,何睿文,韩永和,等.胃肠模拟体外法的生理参数对室内灰尘中邻苯二甲酸酯与磷系阻燃剂的生物有效性的影响[J].环境科学学报, 2016,36(5):1841-1848.
【10】胡庆亮,黄宁宝,王艳,等.模拟胃肠液用Tenax提取法测定多溴联苯醚的生物有效性[J].环境化学, 2014,33(8):1253-1260.
【11】秦静,刘晓宇,刘幸,等.基于体外消化模型的食品中邻苯二甲酸酯生物有效性的测定[J].食品安全质量检测学报, 2013(1):207-210.
【12】陈珊,许宜平,王子健.有机污染物生物有效性的评价方法[J].环境化学, 2011,30(1):158-164.
【13】任超,赵祯,柳金明,等.典型废物回收园区土壤中邻苯二甲酸酯分布与风险评价[J].环境化学, 2018,37(8):1691-1698.
【14】TILSTON E L, GIBSON G R, COLLINS C D. Colon extended physiologically based extraction test (CE-PBET) increases bioaccessibility of soil-bound PAH[J]. Environmental Science & Technology, 2011,45(12):5301-5308.
【15】LEE C M. Environmental organic chemistry, 2nd edition (Schwarzenback, Rene P.; Gschwend, Philip M.; Imboden, Dieter M.)[J]. Journal of Chemical Education, 2003,80(10):1143-1148.
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