全部 标题 作者
关键词 摘要

OALib Journal期刊
ISSN: 2333-9721
费用：99美元
投递稿件

查看量下载量

相关文章

更多...
环境化学  2015 

海洋沉积物中甾醇类物质的气相色谱/质谱方法分析

Keywords: 甾醇,沉积物,气相色谱-质谱联用

Full-Text   Cite this paper   Add to My Lib

Abstract:

应用超声提取技术,结合硅胶-中性氧化铝柱层析净化分离,BSTFA+1%TMCS衍生,及气相色谱-质谱定性定量技术,建立了海洋表层沉积物中8种甾醇类化合物的定量分析方法.实验采用正交实验优化了提取过程中提取剂种类、试剂体积和超声时间,同时对比并优化了柱层析淋洗液的配比、用量以及衍生剂的用量.结果表明,50mL二氯甲烷/甲醇(V/V,21),超声40min,超声3次,总甾醇的萃取率可达99.6%;3g硅胶+2g中性氧化铝层析,35mL二氯甲烷/甲醇(V/V,91)淋洗净化回收最佳;8种甾醇在0—848μg·L-1范围内有良好的线性关系;方法检测限为1.2—2.4ng·g-1.在3种浓度水平0.05、0.1和1.0μg·g-1下,其平均回收率为76.2%—100.9%,相对标准偏差为1.0%—10.3%.应用本方法检测大连湾的3个沉积物样品,8种甾醇的含量在0.079—6.833μg·g-1范围内.本方法的灵敏度高、准确度好,适合用于沉积物样品中甾醇物质的检测要求.

 References

[1]  Volkman J K, Barrett S M, Blackburn S I, et al. Microalgal biomarkers:A review of recent research developments [J]. Organic Geochemistry, 1998, 29 (5/7): 1163-1179
[2]  Volkman J K, Revill A T, Bonham P I,et al. Sources of organic matter in sediments from the Ord River in tropical northern Australia[J]. Organic Geochemistry, 2007, 38(7):1039-1060
[3]  Leonard Y, Jayasinghe, Philip J M, et al. Application of pentafluorophenyldimethylsilyl derivatization for gas chromatography-electron-capture detection of super critically extracted sterols [J]. Journal of Chromatography A, 1998, 809: 109-120
[4]  谢敏浩,裘爱泳,何拥军,等. 甾醇、甾烷醇柱前衍生高效液相荧光分析[J]. 分析化学,2006,34:S131-S134
[5]  马海青,冯环,王旭晨. 渤海湾和胶州湾表层沉积物中甾醇的分布和来源[J]. 海洋科学, 2009,6: 73-79
[6]  Jayasinghe L Y, Marriott P J, Carpenter P D, et al. Application of pentafluorophenyldimethylsilyl derivatization for gas chromatography-electron-capture detection of supercritically extracted sterols[J]. Chromatography A, 1998, 809 (1/2):109-120
[7]  B？rjesson E, Sundin A, Leeming R, et al. New method for determination of fecal sterols in urine using non-chlorinated solvents[J]. Chromatography B, 1998, 713(2):438-442
[8]  彭兴跃,洪华生,李玉桂,等 厦门西海域表层沉积物中甾醇的模糊聚类分析[J]. 环境科学学报,1997, 17(4): 399-405
[9]  段毅,崔明中,马兰华. 南沙海域中大陆坡沉积物中甾醇的地球化学研究[J]. 地球化学,1998,27(1): 4-80
[10]  Li Donghao, Dong Meihua, Shim WJ, et al. Application of pressurized fluid extraction technique in the gas chromatography-mass spectrometry determination of sterols from marine sediment samples [J]. Journal of Chromatography A, 2007, 1160: 64-70
[11]  吕晓霞,翟世奎. 长江口柱状沉积物中甾醇的组成特征及其地球化学意义[J]. 海洋学报, 2006, 28(4):96-107
[12]  Froehner S, Martins R F, Errera M R. Sediments as a potential tool for assessment of sewage pollution in Barigüi River, Brazil [J]. Environmental Monitoring and Assessment, 2009, 157:591-600
[13]  徐恒振,刘星,姚子伟. 粪固醇作为海洋环境中粪便污染指示物的研究[J]. 海洋环境科学, 2010, 29(6):777-780
[14]  Careri M, Elviri L, Mangia A. Liquid chromatography-UV determination and liquid chromatography atmospheric pressure chemical ionization mass spectrometric characterization of sitosterol and stigmasterol in soybean oil [J]. Chromatography A, 2001, 935: 249-257
[15]  Choi S M, Kwan S Y, Wong C M. Studies of coprostanol (5β-Cholestan-3β-ol) in environmental samples by tandem mass spectrometry[J]. Microchemical Journal, 1996, 53(8):54-64
[16]  Leeming R, Ball A, Ashbolt N, et al. Using faecal sterols from humans and animals to distinguish faecal pollution in receiving waters [J]. Water Research, 1996, 30(12):2893-2900

Full-Text

Contact Us

service@oalib.com

QQ:3279437679

WhatsApp +8615387084133