25 - 食品科学技术页

[7]摇 Chen Xiaohong, Zhao Yonggang, Shen Haoyu, et al.
Application of dispersive solid鄄phase extraction and ultra鄄
fast liquid chromatography鄄tandem quadrupole mass spec鄄
trometry in food additive residue analysis of red wine
[J]. Journal of Chromatography A ,2012, 1263:34-42.
[8]摇 庄丽丽. 固相萃取 气相色谱法测定葡萄酒中 16 种有
机磷农药残留 [ J]. 福建分析测试 , 2012, 21 ( 5 ):
11-16.
[9]摇 朱学良, 戚向阳, 岳晶念, 等. 基质固相分散气相色谱
电子捕获检测器测定葡萄酒中 5 种农药残留 [ J]. 分
析化学, 2007,35(2):259-262.
[10]摇 Pecek G, Pavlovic D M, Babic S. Development and val鄄
idation of a SPE鄄GC鄄MS method for the determination of
pesticides in surface water[ J]. International Journal of
Environmental Analytical Chemistry, 2013, 93 ( 12 ):
1311-1328.
[11]摇 Pang Guofang, Cao Yanzhong, Zhang Jinjie, et al. Val鄄
idation study on 660 pesticide residues in animal tissues
by gel permeation chromatography cleanup / gas chroma鄄
tography鄄mass spectrometry and liquid chromatography鄄
tandem mass spectrometry [J]. Journal of Chromatogra鄄
phy A, 2006, 1125(1):1-30.
[12]摇 Kwon H, Lehotay S J, Geis鄄Asteggiante L. Variability
of matrix effects in liquid and gas chromatography鄄mass
spectrometry analysis of pesticide residues after QuECh鄄
ERS sample preparation of different food crops [ J ].
Journal of Chromatography A, 2012, 1270(28): 235 -
245.
[13]摇 Koesukwiwat U, Lehotay S J, Mastovska K, et al. Ex鄄
tension of the QuEChERS Method for Pesticide Residues
in Cereals to FlaxseedsPeanuts, and Doughs[ J]. Jour鄄
nal of Agricultural and Food Chemistry, 2010,58(10):
5950-5958.
[14]摇 章晴,陈士恒 ,杨永坛. 分散固相萃取气相色谱法测
定茶叶中 25 种有机氯与拟除虫菊酯农药残留 [ J].
分析仪器, 2013, (4):16-22.
[15]摇 杜晓婷,周敏, 张剑,等. 蔬菜中甲胺磷等 5 种有机磷
农药残留量的分散液 - 液微萃取 / 气质联用技术检
测[J]. 分析测试学报,2010, 29(7):751-754.
[16]摇 中华人民共和国卫生部; 中华人民共和国农业部 .
GB 2763—2012 食品安全国家标准 ———食品中农药
最大残留限量[S]. 北京:中国标准出版社,2012.
Fast Determination of 52 Pesticide Residues in
Grape Wine by DSPE鄄GC / MS
CHEN Shiheng,摇 ZHANG Qing,摇 SHI Xiaomei,摇 YANG Yongtan * ,摇 YU Weizu
( COFCO Nutrition and Health Research Institute / Beijing Key Laboratory of Nutrition,
Health and Food Safety, Beijing 100020, China)
Abstract: A fast method was developed for determination of 52 pesticides in grape wine by using DSPE
and GC鄄MS. The samples were first extracted using acetonitrile with the addition of vibration and ultra鄄
sound. Then mix adsorbents were used in dispersive solid phase extraction to purify the extracts. After
the high speed centrifugation, nitrogen flushing concentration, and filtration, the samples were detected
by GC / MS using selective ion monitoring (SIM) . Compared with traditional methods, QuEChERS had
advantages in cost and pretreatment speed. The spiked recoveries at three levels of 52 pesticides were in
range of 60% - 110% while the relative standard deviations ( n = 5) were all less 15% . Meanwhile, the
limit of quantity (LOQ) were in the range of 0郾 000 7 - 0郾 032 3 mg / kg. With features such as accuracy
and easy operation, this method could be used to fast determination of 52 pesticides in grape wine without
any special apparatus and also satisfied the requirement of the pesticide routine analysis.
Key words: multiple pesticide residues; dispersive solid phase extraction; grape wine; fast determina鄄
tion
( 责任编辑: 李摇 宁)
22 食品科学技术学报 摇 摇 摇 摇 摇 摇 摇 摇 摇 摇 摇 摇 摇 摇 摇 摇 摇 2014 年 5 月