ASE-UHPLC-MS/MS Determination of 8 Environmental Endocrine Disrupters in Sediments
摘 要
取经前处理后的沉积物样品(5.000 g)与中性氧化铝粉25 g充分混匀,按规定条件用丙酮-甲醇(1+1)混合液进行加速溶剂萃取其中的8种内分泌干扰物。所得萃取液吹氮浓缩至2 mL,加水400 mL并调节pH至3,溶液经HLB固相萃取小柱净化。小柱用氮气吹干后,用丙酮8 mL洗脱。洗脱液经处理后进行超高效液相色谱-串联质谱分离。以BEH C18柱为固定相,以不同体积比的甲醇和0.1%(体积分数)氨水溶液为流动相进行梯度洗脱。在质谱分析中,采用电喷雾负离子源和多反应监测模式。8种化合物的质量浓度在2.0~100.0 μg·L-1范围内呈线性,检出限(3s)在0.03~0.05 μg·kg-1之间。按标准加入法在3个浓度水平上进行回收试验,回收率在62.8%~104%之间,测定值的相对标准偏差(n=6)在2.8%~15%之间。
Abstract
The pretreated sediment sample (5.000 g) was mixed thoroughly with neutral Al2O3 (25 g), and 8 endocrine disrupters in the sample were separated by ASE as described with a mixture of acetone and methanol (1+1). The extract was concentrated to 2 mL by N2-blowing, 400 mL of water were added and acidity of the solution was adjusted to pH 3. The solution was then purified by passing through HLB-SPE column. After drying the column by N2-blowing, it was eluted with 8 mL of acetone. The treated eluate was separated by UHPLC using BEH C18 column as the stationary phase, and mixtures of methanol and 0.1% (φ) ammonia solution, mixed in various volumic ratios, as mobile phase in gradient elution. ESI- and MRM were adopted in MS. Linear relationships between values of peak area and mass concentration of 8 compounds were found in the range of 2.0-100.0 μg·L-1, with detection limits (3s) in the range of 0.03-0.05 μg·kg-1. Test for recovery was made by standard addition method at 3 concentration levels, giving results in the range of 62.8%-104%, with RSDs (n=6) ranged from 2.8% to 15%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201704010
所属栏目 工作简报
基金项目 江苏省环境监测基金项目(1305)
收稿日期 2016/3/23
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备注张蓓蓓(1982-),女,江苏东台人,高级工程师,硕士,主要从事环境中有毒有害污染物监测工作。E-mail:zbb@jshb.gov.cn
引用该论文: ZHANG Bei-bei,ZHAO Yong-gang. ASE-UHPLC-MS/MS Determination of 8 Environmental Endocrine Disrupters in Sediments[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(4): 418~424
张蓓蓓,赵永刚. 加速溶剂萃取-超高效液相色谱-串联质谱法测定沉积物中的8种环境内分泌干扰物[J]. 理化检验-化学分册, 2017, 53(4): 418~424
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【9】ISOBE T, SERIZAWA S, HORIGUCHI T, et al. Horizontal distribution of steroid estrogens in surface sediments in Tokyo Bay[J]. Environmental Pollution, 2006,144(2):632-638.
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【14】雷炳莉,黄圣彪,王东红,等.温榆河沉积物中6种雌激素的存在状况[J].环境科学, 2008,29(9):2419-2424.
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