作者：克选

作者单位：甘肃省张掖市环境监测站, 甘肃 张掖 734000

关键词：加速溶剂萃取;气相色谱质谱;土壤;双酚A

摘要：

建立加速溶剂萃取后利用气相色谱-质谱法测定土壤中双酚A的检测方法。样品前处理采用加速溶剂萃取,经硅胶柱净化,以HP-5MS色谱柱,采用气相色谱-质谱联用全扫描和选择离子扫描进行分析。结果表明:双酚A在0.1~10.0 mg/L的质量浓度范围内,线性良好,相关系数为0.999 3;方法检出限为0.01 mg/kg(S/N=3)。在0.1,1.0,10 mg/kg这3个加标水平下,样品的平均回收率为82.5%~101.7%,相对标准偏差(RSD)3.3%。该方法简便快速,灵敏度及准确度高,可用于土壤中双酚A的分析测定。

Determination of bisphenol-A in soil using GC-MS combined with accelerated solvent extraction

KE Xuan

Gansu Province Environmental Monitoring Station of Zhangye City, Zhangye 734000, China

Abstract: A method is developed to determine bisphenol-A in soil with gas chromatography- mass spectrometry (GC-MS) after accelerated solvent extraction. It is carried out by the following steps: prepare samples via accelerated solvent extraction, purify the prepared sample on a silica gel column, further separated it on an HP-5MS column, and then analyze it via GC-MS full scanning and selective ion monitoring(SIM). The calibration curves of bisphenol-A showed a good linearity and the correlation coefficient and detection limit(S/N=3) thereof are 0.999 3 and 0.01 mg/kg respectively, under the optimized conditions namely ranging from 0.1 mg/L to 10.0 mg/L. The average recovery rate of the sample is within 82.5%-101.7% at the spiked levels of 0.1, 1.0, 10.0 mg/kg, with the relative standard deviation(RSDs) lower than 3.3%. This method is simple and rapid with high sensitivity and resolution. It can be used to determine the amount of bisphenol-A in soil.

Keywords: accelerated solvent extraction;GC-MS;soil;bisphenol-A

2016, 42(3): 45-47,63  收稿日期: 2015-07-18;收到修改稿日期: 2015-09-25

基金项目: 

作者简介: 克选(1983-),男,甘肃民乐县人,工程师,主要从事环境监测工作。

参考文献

[1] 章思归. 实用精细化学品手册:有机卷[M]. 北京:化学工业出版社,1996:398.
[2] 秦定霞,崔毓桂,刘嘉茵. 双酚A对生殖系统的影响及其作用机制[J]. 国际生殖健康/计划生育杂志,2010,29(1):26-29.
[3] GROFF T. Bisphenol A:invisible pollution[J]. Wolters Kluwer Health,2010,22(4):1040-8703.
[4] HIROI H, TSUTSUMI O, FAKEUCHJ T, et al. Differences in serum bisphenol a concentrations in p remenopausal normal women and w omen with endometrial hyperplasia[J]. Endocr J,2004,51(6):595-600.
[5] SUGIURA O M, OZAKI Y, SONTA S, et al. Exposure to bisphenol A is associated with recurrent miscarriage[J]. Human Reproduction,2005,20(8):2325-2329.
[6] PRINS G S, TANG W Y, BELMONTE J, et al. Developmental exposure to bisphenol A increases prostate cancer susceptibility inadultrats:Epigenetic mode of action is implicated[J]. Fertility and Sterility,2008,89(2,11):41-42.
[7] HO S M, TANG W Y, BELMONTE J, et al. Developmental exposure to estradiol or bisphenol A increases susceptibility to prostate carcingenesis and epigenetically regulates phosphodiesterase4[J]. Cancer Research,2006(66):5624-5632.
[8] VANDENBERG L N, HAUSER R, MARCUS M, et al. Human exposure to bisphenol A (BPA)[J]. Reproductive Toxicology,2007,24(2):139-177.
[9] CRAIG D R, BROWN E, CRAFT J A, et al. Effects of sewage effluent and ethynyl oestradiol upon molecular markers of oestrogenic exposure, maturation and reproductive success in the sand goby[J]. Aquatic Toxicology,2003(62):119-134.
[10] KUURANNE T, VAHERMO M, LEINONEN A, et al. Electrospray and atmospheric pressure chemical ionization tandem mass spectrometric behavior of eight anabolic steroid glucuronides[J]. J Am Soc Mass Spectrom,2000,11(8):720-730.
[11] 张亦农,刘欣,张长久,等. 雄烯二酮特征代谢物的质谱分析[J]. 质谱学报,2001,22(3):76-79.
[12] 崔凯荣,张亦农,刘欣. 人尿中Carphedone的气相色谱-质谱分析[J]. 质谱学报,2004,25(3):166-168.
[13] LEE S T, LAM T J, TAN C H. Increased 21-hydroxylase and Shut down of C (17,20) lyase activities in testicular tissues of the grouper (Epinephelus coioides) during 17α-methyl testosterone-induced sex inversion[J]. Gen Gomp Endocrinol,2002,126(3):298-309.