建立了饲料中6种全氟化合物的聚酰胺固相萃取-超高效液相色谱-串联四极杆质谱分析法。样品采用酸化乙腈提取，在酸性条件下用聚酰胺固相萃取小柱富集，甲醇淋洗净化，5％（ v/v）氨水/甲醇溶液洗脱后采用超高效液相色谱-串联四极杆质谱（UPLC-MS/MS）检测。分析柱为 Acquity BEH C18（100 mm×2.1 mm，1.7μm）；流动相为5 mmol/L乙酸铵-乙腈梯度洗脱；在最佳实验条件下，采用多反应监测负离子模式测定，同位素内标法定量。该方法对6种全氟化合物的检出限均小于0.1μg/kg；对6种饲料及原料的加标回收率为94.2％~108.9％，精密度（ RSD）为1.8％~8.6％（ n=6）；在0.5~25μg/L范围内均呈良好的线性关系，线性回归系数 r﹥0.995。该方法前处理成本低，效果好，适合复杂基质样品的检测。
A method for the determination of six perfluorinated organic compounds( PFCs)in feed has been developed. It is based on polyamide solid-phase extraction( SPE)together with ultra performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS ). The sample was extracted by acidified acetonitrile. The extraction solution was enriched by a poly-amide SPE cartridge under acidic condition,and cleaned-up using methanol,eluted by 5%( v/v)ammonia/methanol solvent and determined by UPLC-MS/MS. The UPLC separation was carried out on an Acquity BEH C18 column(100 mm×2. 1 mm,1. 7 μm). The mobile phases were 5 mmol/L ammonium acetate and acetonitrile with a gradient elution. Under the optimal conditions,the PFCs were analyzed under multiple reaction monitoring( MRM)mode with neg-ative electrospray ionization. The isotope internal standard method was used to determine the six PFCs,and improve the quantitative accuracy. All of the target compounds exhibited good linearity( r﹥0. 995)over a concentration range of 0. 5-25 μg/L. The detection limits of the six PFCs were all smaller than 0. 1 μg/kg. The mean recoveries of the six PFCs were in the range of 94. 2% to 108. 9% with the relative standard deviations( RSDs)of 1. 8%-8. 6%( n=6). The method for the determination of PFCs in feed is low-cost,favorable effect and suitable for the detection of complex matrix samples.
参考文献
| [1] | Li L,Zhao K F,Li Y M,et al. Journal of Environmental Hygiene(李玲,赵康峰,李毅民,等. 环境卫生学杂志), 2013,3(2):167 |
| [2] | Peng S Y,Yan L J,Zhang J,et al. Chinese Journal of Chro-matography(彭思远,严丽娟,张洁,等. 色谱),2012,30 (2):123 |
| [3] | Shi Y L,Pan Y Y,Wang J M,et al. Progress of Chemistry (史亚利,潘媛媛,王杰明,等. 化学进展),2009,21(2/3):369 |
| [4] | Chen J J,Fang K,Hu M Y. Chemical Production and Tech-nology(陈剑君,方凯,胡鸣韵. 化工生产与技术),2011,18 (3):9 |
| [5] | Chen H M,Zhao M. Textile Auxiliaries(陈红梅,赵梅. 印染助剂),2008,25(8):42 |
| [6] | Lin Q. Food Science(林钦. 食品科学),2013,34(10):241 |
| [7] | Ran X R,Zhang Z X,Zhang Z X. Environmental Chemistry (冉小蓉,张政祥,张之旭. 环境化学),2009,28(3):459 |
| [8] | Guo M M,Wu H Y,Li Z X,et al. Chinese Journal of Analyt-ical Chemistry(郭萌萌,吴海燕,李兆新,等. 分析化学), 2013,41(9):1322 |
| [9] | Liu L Z,Guo X D,Fang J,et al. Journal of Instrumental Analysis(刘莉治,郭新东,方军,等. 分析测试学报),2013, 32(7):862 |
| [10] | Wang Y,Kong D Y,Shan Z J,et al. Environmental Chem-istry(王懿,孔德洋,单正军,等. 环境化学),2012,31 (1):113 |
| [11] | Tseng C L,Liu L L,Chen C M,et al. J Chromatogr A, 2006,1105:119 |
| [12] | Wang J M,Shi Y L,Pan Y Y,et al. Chinese Sci Bull,2010, 55(31):3550 |
| [13] | Wang L B,Lü G,Liu S C,et al. Chinese Journal of Analy-sis Laboratory(王利兵,吕刚,刘绍从,等. 分析试验室), 2007,26(2):94 |
| [14] | Yu H P,Rong H,Lu L J,et al. China Dyeing & Finishing Journal(于徊萍,荣会,卢利军,等. 印染),2007(13):37 |
| [15] | Guo R,Cai Y Q,Jiang G B. Environmental Chemistry(郭睿,蔡亚岐,江桂斌. 环境化学),2006,25(6):674 |
| [16] | GB/T 23243-2009 |
| [17] | GB/T 24169-2009 |
| [18] | SN/T 2257-2009 |
| [19] | Ji Y B,Wu H,Lang L. The Proceedings of China Environ-mental Science Society of Academic Annual Meeting. Bei-jing:China Environmental Science Press(季宇彬,吴昊,郎朗. 中国环境科学学会学术年会论文集. 北京:中国环境科学出版社),2010:4135 |
| [20] | Wu J P,Guan Y T,Li M Y,et al. Ecology and Environ-mental Sciences(吴江平,管运涛,李明远,等. 生态环境学报),2010,19(5):1246 |
| [21] | Wang Y,Yang W X,Yamashita N,et al. Chinese Science Bulletin(王媛,杨伟贤,山下信义,等. 科学通报),2008, 53(2):147 |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%