建立了单壁碳纳米管（ SWCNTs）为吸附剂的固相萃取净化-气相色谱-质谱检测茶油中6种邻苯二甲酸酯（PAEs）的分析方法。样品经正己烷稀释，玻璃 SWCNTs SPE小柱净化，GC-MS选择离子监测（SIM）模式测定，外标法定量。对正己烷的稀释体积、吸附材料的类型、SWCNTs 用量、淋洗液用量、洗脱溶剂类型和体积等影响萃取效率的条件进行了优化，得到的最优萃取条件为：正己烷稀释体积为5 mL，SWCNTs 用量为0.6 g，淋洗液为20 mL正己烷，洗脱溶剂为5 mL 甲苯。6种 PAEs 在0.05~1.0 mg/L 范围内线性关系良好，相关系数（ r）均大于0.9999；在0.05~1.0 mg/kg添加范围内，6种目标物的平均回收率为86.4％~111.7％，相对标准偏差为4.2％~10.4％。该方法准确、快速，可满足茶油中6种邻苯二甲酸酯的检测需要。
An analytical method based on solid-phase extraction with single-walled carbon nanotubes( SWCNTs ) as adsorbent was developed for the simultaneous determination of six phthalate acid esters( PAEs)in camellia oil by gas chromatography-mass spectrometry( GC-MS). The samples were diluted by hexane and then cleaned up with a glass SWCNTs solid phase extraction( SPE)column. The PAEs were measured by GC-MS in selected ion monito-ring( SIM)mode,using external standard method for quantitative analysis. The important fac-tors affecting extraction efficiency,such as the dilution volume of hexane,the type of adsor-bent material,the dosage of SWCNTs,the volume of wash solution,the type and volume of elution solution were optimized. The optimal conditions were as follows:the dilution volume of hexane was 5 mL,the dosage of SWCNTs was 0. 6 g,the wash solution was 20 mL hexane,and the elution solution was 5 mL toluene. The six PAEs had a good linear range from 0. 05 mg/L to 1. 0 mg/L,with the correlation coefficients( r)all above 0. 999 9. The average recoveries of the six targets in spiked camellia oil( from 0. 05 mg/kg to 1. 0 mg/kg ) ranged from 86. 4% to 111. 7% with the relative standard deviations ( RSDs ) from 4. 2% to 10. 4%. The developed method is accurate,quick and suitable for the determination of the six PAEs in camellia oil.
参考文献
| [1] | Gong H P,Xia A P,Zheng R X,et al. Farm Machinery(龚鸿萍,夏爱萍,郑睿行,等. 农业机械),2012(33):58 |
| [2] | Ma L,Chen Y Z. Chinese Agricultural Science Bulletin(马力,陈永忠. 中国农学通报),2009,25(8):82 |
| [3] | Long Q Z,Huang Y H,Zhong H Y,et al. Journal of the Chi-nese Cereals and Oils Association(龙奇志,黄永辉,钟海雁,等. 中国粮油学报),2009,24(1):70 |
| [4] | Fasano E,Bono-Blay F,Cirillo T,et al. Food Control, 2012,27:132 |
| [5] | Marega M,Grob K,Moret S,et al. J Chromatogr A,2013, 1273:105 |
| [6] | Yao W R,Yu Y,Yan W,et al. China Oils and Fats(姚卫蓉,俞晔,阎微,等. 中国油脂),2010,35(6):38 |
| [7] | Yang Y C,Zhang M M,Sun Y M,et al. Journal of the Chi-nese Cereals and Oils Association(杨艺超,张明明,孙远明,等. 中国粮油学报),2012,27(6):110 |
| [8] | Zheng X H,Lin L Y,Fang E H,et al. Chinese Journal of Chromatography(郑向华,林立毅,方恩华,等. 色谱), 2012,30(1):27 |
| [9] | De Orsi D,Gagliardi L,Porrà R,et al. Anal Chim Acta, 2006,555:238 |
| [10] | Li R W,Cheng G H,Wang T,et al. China Brewing(李仁伟,成桂红,王涛,等. 中国酿造),2011(7):180 |
| [11] | Holadova K,Prokupkova G,Hajslova J,et al. Anal Chim Acta,2007,582:24 |
| [12] | Zhang C Y,Wang H,Zhang X H,et al. Chinese Journal of Chromatography(张春雨,王辉,张晓辉,等. 色谱),2011, 29(12):1236 |
| [13] | Wang P G,Gao M X,Cheng G,et al. Food Science(王鹏功,高明星,程刚,等. 食品科学),2012,33(18):246 |
| [14] | Hu Y C,Li M Y,Xu J,et al. Journal of Food Science and Biotechnology(胡银川,李明元,徐锦,等. 食品与生物技术学报),2011,30(4):583 |
| [15] | Chen Z M,Xu X F,Ding Y P,et al. Chinese Journal of Health Laboratory Technology(陈志民,徐晓枫,丁永萍,等. 中国卫生检验杂志),2013,23(2):304 |
| [16] | Xu D M,Deng X J,Fang E H,et al. J Chromatogr A, 2014,1324:49 |
| [17] | Lijima S. Nature,1991,354:56 |
| [18] | Kroto H W,Heath J R,O′Brien S C,et al. Nature,1985, 318:162 |
| [19] | Li H F,Yang H Y,Zhang Y,et al. Chinese Journal of Chro-matography(李海芳,杨红云,张英,等. 色谱),2014,32 (4):413 |
| [20] | Zhang B T,Zheng X X,Li H F,et al. Anal Chim Acta, 2013,784:1 |
| [21] | Zhang F,Li Z H,Huang Y Y,et al. Food &Machinery(张帆,李忠海,黄媛媛,等. 食品与机械),2013,29(5):87 |
| [22] | Pyrzynska K. Chemosphere,2011,83:1407 |
| [23] | He S W,Huang Z P,Zhu Y. Chinese Journal of Chromatog-raphy(何世伟,黄忠平,朱岩. 色谱),2013,31(12):1146 |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%