基于PA6纳米纤维膜固相萃取-液相色谱法检测牛奶中的邻苯二甲酸酯

高等学校化学学报 ›› 2010, Vol. 31 ›› Issue (4): 690.

基于PA6纳米纤维膜固相萃取-液相色谱法检测牛奶中的邻苯二甲酸酯

殷雪琰 , 许茜1,2, 吴淑燕1, 王敏1, 顾忠泽2

1. 东南大学公共卫生学院, 南京 210009;
2. 东南大学生物电子学国家重点实验室, 南京 210096

收稿日期:2009-07-20 出版日期:2010-04-10 发布日期:2010-04-10
通讯作者: 许茜, 女, 副教授, 主要从事食品和药品分析研究. E-mail: q_xu@163.com
基金资助:
国家自然科学基金(批准号: 50533030)和江苏省科技计划项目(批准号: BK2006509)资助.

Determination of Phthalate Esters in Commercial Milk Samples Using PA6 Nanofibers Mat-based Solid-phase Extraction Coupled with Liquid Chromatography

YIN Xue-Yan1, XU Qian1,2*, WU Shu-Yan1, WANG Min1, GU Zhong-Ze2

1. School of Public Health, Southeast University, Nanjing 210009, China;
2. State Key Laboratory of Bioelectronics, Southeast University, Nanjing 210096, China

Received:2009-07-20 Online:2010-04-10 Published:2010-04-10
Contact: XU Qian. E-mail: q_xu@163.com
Supported by:
国家自然科学基金(批准号: 50533030)和江苏省科技计划项目(批准号: BK2006509)资助.

摘要/Abstract

摘要：

采用静电纺丝法制备了聚酰胺6(PA6)纳米纤维膜, 结合固相萃取技术-液相色谱法(HPLC-UV)检测了市售牛奶样品中的6种邻苯二甲酸酯(PAEs)的含量. 对影响实验的各种因素, 如提取溶剂的种类及用量、超声时间、洗脱溶剂的种类及用量、纳米纤维膜的用量、pH及过样速度等进行了考察. 在最优化条件下, 邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸丁基苄酯(BBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基己)酯(DEHP)和邻苯二甲酸二正辛酯(DOP)的检出限分别为0.02, 0.01, 0.05, 0.05, 0.10和0.25 ng/mL. 将该方法应用于不同品牌不同包装牛奶样品的检测, 只需2.5 mg PA6纳米纤维膜, 即可完全萃取样品中的PAEs, 相对标准偏差(RSD)小于5.82%, 回收率为93.40%~104.83%. 该方法测定牛奶中PAEs环境雌激素, 检出限低, 灵敏度高, 结果准确可靠, 重现性好.

关键词: 邻苯二甲酸酯; PA6纳米纤维膜; 高效液相色谱-紫外检测; 固相萃取; 牛奶

Abstract:

A new method for simultaneous determnation of six phthalate esters in commercial milk was deve-loped by the combination of latest proposed PA6 nanofibers mat-based solid-phase extraction with high-perfor-mance liquid chromatography-ultraviolet detector(HPLC-UV). Conditions for obtaining optimum extraction efficiency such as extraction solvents and its volume, extraction time, eluant and its volume, amount of adsorbent, pH, flow rate of sample were investigated and optimized in detail. Under optimized conditions, the detection limits found for dimethyl phthalate(DMP), diethyl phthalate(DEP), butylbenzyl phthalate(BBP), dibutyl phthalate(DBP), diethyl hexylphthalate(DEHP) and dioctyl phthalate(DOP) were 0.02, 0.01, 0.05, 0.05, 0.10 and 0.25 ng/mL, respectively. The proposed method was applied to the analysis different brands and packaging of milk samples. PAEs in commercial milk samples can be completely extracted by 2.5 mg PA6 nanofiber mat. The satisfactory spiked recoveries were obtained in the range of 93.40%—104.83% with relative standard deviation(RSD) of below 5.82% were achieved. The main advantages of the method are low detection limits, high sensitivity and selectivity and the results are accurate and reliable, reproducible.

Key words: Phthalate ester; PA6 nanofibers mat; High-performance liquid chromatography ultraviolet detector(HPLC-UV); Solid-phase extraction; Milk

TrendMD:

殷雪琰 , 许茜1,2, 吴淑燕1, 王敏1, 顾忠泽2. 基于PA6纳米纤维膜固相萃取-液相色谱法检测牛奶中的邻苯二甲酸酯. 高等学校化学学报, 2010, 31(4): 690.

YIN Xue-Yan1, XU Qian1,2*, WU Shu-Yan1, WANG Min1, GU Zhong-Ze2. Determination of Phthalate Esters in Commercial Milk Samples Using PA6 Nanofibers Mat-based Solid-phase Extraction Coupled with Liquid Chromatography. Chem. J. Chinese Universities, 2010, 31(4): 690.

参考文献

[1]Castillo M., Oubina A., Barcelo D.. Environ. Sci. Technol.[J], 1999, 32: 2180—2184
[2]LIU Zhen-Ling(刘振岭), XIAO Chun-Hua(肖春华), WU Cai-Ying(吴采樱), et al.. Chinese Journal of Chromatography(色谱)[J] ,2000, 18: 568—570
[3]DING Peng(丁鹏), ZHAO Xiao-Song(赵晓松), LIU Jian-Feng(刘剑峰). Journal of Jinlin Agricultural University(吉林农业大学学报)[J] , 1999, 21(3): 119—123, 128
[4]LI Xiang-Li(李向丽), LIN Li(林里), ZOU Shi-Chun(邹世春), et al.. Chinese J. Anal. Chem.(分析化学)[J], 2006, 34(3): 325—328
[5]LI Min-Xia(李敏霞), WU Jing-Hong(吴京洪), ZENG Wei(曾玮), et al.. Chinese J. Anal. Chem.(分析化学)[J], 2006, 34(8): 1172—1174
[6]Mori S.. J. Chromatogr. B[J], 1976, 129: 53—60
[7]Li X. J., Zeng Z. R., Chen Y., et al.. Talanta[J], 2005, 63(4): 1013—1019
[8]Bartolome L., Cortazar E., Raposo J. C., et al.. J. Chromatogr. A[J], 2005(2), 1068: 229—236
[9]Batlle R., Nerin C.. J. Chromatogr. A[J], 2004, 1045(1/2): 29—35
[10]Cortazar E., Zuloaga O., Sanz J., et al.. J. Chromatogr. A[J], 2002, 978(1/2): 165—175
[11]Vamvakaki V., Fouskaki M., Chaniotakis N.. Analytical Letters[J], 2007, 40(12): 2271—2287
[12]Guo G. S., He C. N., Wang Z. H., et al.. Talanta[J], 2007, 72(5): 1687—1692
[13]Moller K., Kobler J., Bein T.. Journal of Materials Chemistry[J], 2007, 17(7): 624—631
[14]Klabunde K. J.. Nanoscale Material in Chemistry[M], New York: Wiley-Interscience, 2001
[15]Smith J. E., Medley C. D., Tang Z., et al.. Anal. Chem.[J], 2007, 79(8): 3075—3082
[16]Yoshimatsu K., Ye L., Stenlund P., et al.. Biosensors and Bioelectronics[J], 2008, 23(7): 1208—1215
[17]Li J. D., Zhao X. L., Shi Y. L., et al.. J. Chromatogr. A[J], 2008, 1180(1/2): 24—31
[18]Gibson P., Schreuder-Gibson H., Rivin D.. Colloids and Surface A: Physicochemical and Engineering Aspects[J], 2001, 187: 469—481
[19]Kang X. J., Pan C., Xu Q., et al.. Analytica Chimica Acta[J], 2007, 587(1): 75—81
[20]Bortolato S. A., Arancibia J. A., Escandar G. M.. Analytica Chimica Acta[J], 2008, 613(2): 218—227
[21]XU Xiang-Hua(徐向华), FANG Xiao-Ming(方晓明), DING Zhuo-Ping(丁卓平), et al.. Chemistry Online(化学通报)[J], 2008, 6: 420—424
[22]Yang Liu(杨柳). The study of Determination Method about Enriromental Hormone Phthalic Acid Ester in Milk, Cow Feed and Organs[D], Beijing University of Chemical Technology, 2008
[23]Sorensen L. K.. Rapid Commun. Mass Spectrom[J], 2006, 20(7): 1135—1143
[24]Maragou N. C., Lampi E. N., Thomaidis N. S., et al.. J. Chromatogr. A[J], 2006, 1129(2): 165—173
[25]中华人民共和国国家标准, 食品中邻苯二甲酸酯的测定. GB/T 21911—2008