College of Chemistry, Jilin University, 2699 Qianjin Street, Changchun 130012, China.
J Chromatogr A. 2011 Aug 5;1218(31):5047-54. doi: 10.1016/j.chroma.2011.05.088. Epub 2011 Jun 1.
The multiwall carbon nanotubes (MWCNTs)-based matrix solid phase dispersion (MSPD) was applied for the extraction of hormones, including 17-α-ethinylestradiol, 17-α-estradiol, estriol, 17-β-estradiol, estrone, medroxyprogesterone, progesterone and norethisterone acetate in butter samples. The method includes MSPD extraction of the target analytes from butter samples, derivatization of hormones with heptafluorobutyric acid anhydride-acetonitrile mixture, and determination by gas chromatography-mass spectrometry. The mixture containing 0.30 g graphitized MWCNTs and 0.10 g MWCNTs was selected as absorbent. Ethyl acetate was used as elution solvent. The elution solvent volume and flow rate were 12 mL and 0.9 mL min(-1), respectively. The recoveries of hormones obtained by analyzing the five spiked butter samples were from 84.5 to 111.2% and relative standard deviations from 1.9 to 8.9%. Limits of detection and quantification for determining the analytes were in the range of 0.2-1.3 and 0.8-4.5 μg kg(-1), respectively. Compared with other traditional methods, the proposed method is simpler in the operation and shorter in the sample pretreatment time.
基于多壁碳纳米管（MWCNTs）的基质固相分散（MSPD）被应用于从黄油样品中提取激素，包括 17-α-乙炔基雌二醇、17-α-雌二醇、雌三醇、17-β-雌二醇、雌酮、醋酸甲地孕酮、孕酮和炔诺酮。该方法包括从黄油样品中用 MSPD 提取目标分析物，用七氟丁酸酐-乙腈混合物对激素进行衍生化，然后用气相色谱-质谱法进行测定。选择含有 0.30 g 石墨化 MWCNTs 和 0.10 g MWCNTs 的混合物作为吸附剂。乙酸乙酯被用作洗脱溶剂。洗脱溶剂的体积和流速分别为 12 mL 和 0.9 mL min(-1)。通过分析五个加标黄油样品得到的激素回收率为 84.5%至 111.2%，相对标准偏差为 1.9%至 8.9%。用于测定分析物的检出限和定量限分别为 0.2-1.3 和 0.8-4.5 μg kg(-1)。与其他传统方法相比，该方法在操作上更简单，样品预处理时间更短。
