建立了化妆品中三聚氰胺的亲水作用色谱-质谱联用(HILIC-MS/MS)检测方法.样品经三氯乙酸溶液提取(脂溶性样品再经正己烷萃取)后,用混合型阳离子交换(MCX)反相固相萃取柱富集净化,用5 mmol/L 乙酸铵水溶液(含0.1%甲酸)和乙腈作为流动相,以梯度洗脱方式在ZIC-HILIC色谱柱上实现分离,以电喷雾离子源正离子(ESI+)模式进行质谱分析.三聚氰胺在0.02~0.5 mg/L 范围内呈良好线性关系,相关系数为 0.9985;方法的检出限(LOD,信噪比(S/N)≥3)为5.0 μg/kg,定量限(LOQ,S/N>10)为20.0 μg/kg;在0.01~0.1 mg/kg 添加浓度范围内,三聚氰胺的平均回收率为84.7%~93.4% ,相对标准偏差为4.5%~8.4% .该方法能满足化妆品中三聚氰胺残留量的检测.
参考文献
[1] | Yan L J,Wu M,Zhang Z G,et al.Chinese Journal of Chromatography (严丽娟,吴敏,张志刚,等.色谱),2008,26(6):759 |
[2] | Zhu L P,Sun J Q,Yan S G.China Dairy Industry (朱丽萍,孙建全,颜世敢.中国乳品工业),2010,38(3):51 |
[3] | Liang M Z.Guangdong Chemical Industry (梁楣珍.广东化工),2009,36(12):104 |
[4] | Sun W H,Leng K L,Xing L H,et al.Chinese Journal of Analysis Laboratory (孙伟红,冷凯良,邢丽红,等.分析试验室),2009,28(10):59 |
[5] | Li X Q,Zhang Q H,Quan C,et al.Journal of Instrumental Analysis (李秀琴,张庆合,全灿,等.分析测试学报),2009,28(11):1260 |
[6] | Huang F,Huang X L,Wu H Q,et al.Journal of Instrumental Analysis (黄芳,黄晓兰,吴惠勤,等.分析测试学报),2008,27(3):313 |
[7] | Li F G,Yao W Q,Su M,et al.Chinese Journal of Chromatography (李锋格,姚伟琴,苏敏,等.色谱),2009,27(2):233 |
[8] | Cai Q R,Ouyang Y Y,Qian Z J,et al.Chinese Journal of Chromatography (蔡勤仁,欧阳颖瑜,钱振杰,等.色谱),2008,26(3):339 |
[9] | Rao Q X,Tong J,Wang J F,et al.Feed Industry (饶钦雄,童敬,王金芳,等.饲料工业),2009,30(11):34 |
[10] | FDA.Laboratory Information Bulletin No.4421 of U.S.Food and Drug Administration.(2008-10-06)[2010-07-02].http:/ /www.cfsan.fda.gov/ ~frf/lib4421.html |
[11] | Li R P,Huang J X.Progress in Chemistry (李瑞萍,黄骏雄.化学进展),2006,18(11):1508 |
[12] | Zhao T G.Hygienic Standard for Cosmetics.2007 ed.Beijing:Military Medical Science Press (赵同刚.化妆品卫生规范.2007 版.北京:军事医学科学出版社),2007:165 |
[13] | Ma Q,Wang C,Bai H,et al.Chinese Journal of Chromatography (马强,王超,白桦,等.色谱),2009,27(6):856 |
[14] | Sun X Y,Li Y,Liu L,et al.Chinese Journal of Chromatography (孙小颖,李英,刘丽,等.色谱),2009,27(6):852 |
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