Abstract
A novel method for the determination of vanillin in powdered milk by liquid-liquid extraction - solidification of acceptor phase droplet-reextraction combined with gas chromatography/mass spectrometry(GC/MS) was developed. The sample was extracted with ether and the supernatant was cleaned up using 0.01 mol/L 100 μL sodium hydroxide and the residue was reextracted with dichloromethane. The detection of vanillin was carried out by GC—MS in selected ion monitoring(SIM) mode and external standard method was used for quantitative determination. Under the optimum conditions, the linear range of the method was from 0.20 to 10.0 μg/mL and the linear correlation coefficient (R) was higher than 0.999 5. The limit of detection (S/N=3) was 0.004 mg/kg. The relative standard deviation of the method was less than 6.83% with the recovery values ranging from 82.0% to 98.0%. The proposed method which is very simple, rapid and highly sensitive can meet the needs of determination of vanillin in powdered milk.
Publication Date
4-28-2015
First Page
98
Last Page
101,105
DOI
10.13652/j.issn.1003-5788.2015.02.020
Recommended Citation
Jianhui, ZHANG; Sha, LI; Hui, HUANG; and Lixin, XIA
(2015)
"Determination of vanillin in powdered milk by liquid-liquid extraction-solidification of acceptor phase-reextraction-gas chromatography/mass spectrometry,"
Food and Machinery: Vol. 31:
Iss.
2, Article 20.
DOI: 10.13652/j.issn.1003-5788.2015.02.020
Available at:
https://www.ifoodmm.cn/journal/vol31/iss2/20
References
[1] 邱萍,倪永年.微分脉冲伏安法测定食品中的香兰素［J］.南昌大学学报(理科版),2002,26(2):124～127.
[2] 张国文,倪永年.多元校正—光度法同时测定食品中的香兰素和乙基麦芽酚［J］.分析科学学报,2005,21(1):20～23.
[3] 景丽杰,韩伟.用反相高效液相色谱法测定香兰素含量［J］.食品科学,2006,27(4):205～207.
[4] 赵志红,张逢秋.反相高效液相色谱法同时测定食品中香兰素、乙基麦芽酚的含量［J］.食品科技,2006（12）:136～138.
[5] 韩超,刘滨.液相色谱—串联质谱法同时测定婴幼儿配方奶粉中4种香料［J］.分析测试学报,2014,33（2）:208～211.
[6] Lowri S,Jager D,Gracia A.Comparison of head-space SPME—GCMS and LCMS for the detection and quantification of coumarin,vanillin and ethyl vanillin in vanilla extract products［J］.Food Chemistry,2008,107(4):1 701～1 709.
[7] 欧菊芳,顾秀英.气相色谱法测定婴幼儿配方奶粉中香兰素和乙基香兰素［J］.江西科学,2011,29(1):23～25.
[8] 韩双,杨金宝.气相色谱—质谱/选择离子法测定牛奶中的香兰素［J］.中国乳品工业,2008,36(8):53～55.
[9] 乙小娟,朱加叶.气相色谱—质谱法测定巧克力中香兰素、特丁基对苯二酚、咖啡因［J］.理化检验(化学分册),2009(12):1 404～1 406.
[10] Zanjani M R K,Yamini Y,Shariati S.A new liquid-phase microextraction method based on solidification of floating organic drop［J］.Analytica. Chimica. Acta, 2007, 585(2): 286～293.
[11] 翦英红,胡艳.分散液液微萃取—上浮溶剂固化/高效液相色谱法测定沉积物中的十溴联苯醚［J］.分析化学,2010,38(1):62～66.
[12] 王宇,邹晓莉.混合萃取剂—悬浮固化分散液相微萃取测定尿中的苯巯基尿酸［J］.分析化学,2013,41(5):749～753.
[13] Zhang Jing-Wen,Ke Xiao-jing.Development of dispersive liquid- liquid microextraction based on solidification of floating organic drop for determination of trace cobalt in water samples［J］.Journal of the chinese Chemical Society,2011,58(7):911～918.
[14] Zhang Jing-Wen,Wang Yu-kun.Development of dispersive liquid- liquid microextraction based on solidification of floating organic drop for determination of trace lead in water samples［J］.CLEAN-Soil,Air,Water,2011,39（12）:1 095～1 098.
[15] 石慧,夏丹.分散液液微萃取—反萃取—接受相固化—高效液相色谱法测定减肥茶中的西布曲明［J］.分析化学,2013,41(9):1 444～1 448.