HPLC Determination of 6 Phthalates in Soil and Evaluation of Its Biological Availability
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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.
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Keywords:
- HPLC /
- phthalate /
- biological availability /
- soil
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