作者：林钦1, 黄红霞1, 张莉2, 严恒2, 李道霞3, 刘美3, 李晓瑜4, 黄瑛3
作者单位：1. 福建省产品质量检验研究院, 福建 福州 350002;
2. 湖北省食品质量安全监督检验研究院, 湖北 武汉 430070;
3. 四川省食品药品检验检测院, 四川 成都 610097;
4. 国家食品药品监督管理总局, 北京 100053
关键词：二甲基黄;二乙基黄;高效液相色谱-三重四级杆质谱;豆制品
摘要：
建立一种同时测定豆制品中二甲基黄、二乙基黄的高效液相色谱-三重四级杆质谱（HPLC-MS/MS）方法。对提取溶剂及色谱条件进行优化，粉碎后的样品经乙腈提取，提取液以HPLC-MS/MS测定，外标法定量。二甲基黄、二乙基黄在3 min内流出并完全分离，两者在0.05~10 g/L范围内相关系数r2均大于0.999，二甲基黄在0.5~50 g/kg的加标回收率为90.0%~93.4%，RSD为0.5%~5.1%，二乙基黄在0.5~50 g/kg水平的加标回收率在84.6%~93.8%，RSD为1.1%~4.6%，检出限两者均为0.2 g/kg。该方法操作简捷、准确度和精密度高，适用于豆制品中二甲基黄、二乙基黄的检测。
Simultaneous determination of methyl yellow and ethyl yellow in soy products by high performance liquid chromatography-tandem mass spectrometry
LIN Qin1, HUANG Hongxia1, ZHANG Li2, YAN Heng2, LI Daoxia3, LIU Mei3, LI Xiaoyu4, HUANG Ying3
1. Fujian Inspection and Research Institute for Product Quality, Fuzhou 350002, China;
2. Hubei Provincial Institute for Food Supervision and Test, Wuhan 430070, China;
3. Sichuan Institute for Food and Drug Control, Chengdu 610097, China;
4. China Food and Drug Administration, Beijing 100053, China
Abstract: To establish a method for determination of methyl yellow and ethyl yellow in soy products using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). According to the optimization of extraction solvent and chromatographic conditions, the samples were extracted by acetonitrile and determined by HPLC-MS/MS using external standard method. Methyl yellow and ethyl yellow were separated completely within 3min. The linearity of methyl yellow and ethyl yellow was 0.05-10 μg/L with correlation coefficients(r2) above 0.999. Recoveries ranged from 90.0% to 93.4% for methyl yellow at spiked levels ranging from 0.5 μg/kg to 50 μg/kg, and the relative standard deviations(RSDs) were in the range of 0.5%-5.1%. As for ethyl yellow, recoveries were 84.6%-93.8% at spiked levels ranging from 0.5 μg/kg to 50 μg/kg, and the RSDs were 1.1%-4.6%. The limits of detection were 0.2 μg/kg. The method is rapid, simple, accurate and sensitive. It is suitable for determination of methyl yellow and ethyl yellow in soy products.
Keywords: methyl yellow;ethyl yellow;HPLC-MS/MS;soy products
2017, 43(1): 55-58 收稿日期: 2016-05-21;收到修改稿日期: 2016-07-18
基金项目:
作者简介: 林钦(1970-),男,福建福州市人,高级工程师,博士,主要从事食品理化检验工作。
参考文献
[1] 王春英,刘福德,王娟. 对二氨基偶氮苯及其衍生物的合成与表征[J]. 天津理工大学学报,2010(6):79-81.
[2] 陈世骢,钱挹芬,甘品珍,等. 取代(4-氨基-1-萘偶氮)苯和取代[4-(二乙氨基乙基氨基)-1-萘偶氮]苯类的合成[J]. 药学学报,1966(1):30-37.
[3] WANG Y P, ZHANG S, SUN S M, et al. Ultrafast dynamics of trans-4-diethylaminoazobenzene studied by femtosecond transient absorption spectroscopy[C]//中国化学会.第29届学术年会摘要集——第39分会:化学动力学0657.3. 北京:中国化学会,2014:50.
[4] 李北泉,徐晓利. 二甲氨基偶氮苯诱发大白鼠肝癌形成过程中染色质非组蛋白变化的观察[J]. 中山医学院学报,1983(Z1):1-9.
[5] WU Z Q, YANG S, LIAO W Y, et al. Novel amphiphilic fluorescent graft copolymer:synthesis, characterization and encapsulation of a hydrophobic agent[J]. Chinese Journal of Polymer Science,2006(3):315-321.
[6] 王菡,储晓刚,曹远银. 肉制品中非法添加色素的高效液相色谱快速检测方法[J]. 现代科学仪器,2011(135):90-95.
[7] 吴敏,林建忠,邹伟,等. 高效液相色谱法同时测定食品中对位红和苏丹色素等8种脂溶性染料[J].分析测试学报,2006,25(3):74-76.
[8] 韩劲松,徐明霞,陈湛. 高效液相色谱法测定食品中苏丹红的研究[J]. 中国热带医学,2006,6(7):1245-1246.
[9] 喻凌寒,宋之光,苏流坤,等. 高效液相色谱-离子阱质谱联用测定食品中7种苏丹红类染料[J]. 质谱学报,2006(4):221-225.
[10] MAZZOTTI F, DONNA L D, MAIUOLO L, et al. Assay of set all sudan azodye (I, Ⅱ, Ⅲ, IV and Para-Red) contaminating agents by liquid chromatography-tandam mass spectrometry and isotope dilution methodlogy[J]. J Agric Food Chem,2007(56):63-67.
[11] CALBIANI F, CAERI M, ELVIRI L, et al. Accurate mass measurements for the confirmation of Sudan azo-dyes in hot chilli products by capillary liquid chromatography-electrospray tandem quadrupole orthogonal-acceleretion time of flight mass spectrometry[J]. J Chromatogr A,2004(1058):127-135.
[12] 张协光,曾泳艇,黎永乐. 固相萃取-超高效液相串联质谱同时测定食品中苏丹橙G、二甲基黄、苏丹黑B[J]. 广东化工,2012,39(1):109-110.
[13] 廖梅东,杭义萍. GC-MS与HPLC/DAD联用对纺织品中4-氨基偶氮苯的测定[J]. 分析测试学报,2010(8):846-849.
