建立了高效液相色谱/光化学反应器/荧光检测器测定茶叶中黄曲霉毒素B1的方法。用乙腈水溶液（V∶V=86∶14）提取黄曲霉毒素B1,提取液经净化柱和黄曲霉毒素B1免疫亲和柱净化,高效液相色谱测定。在黄曲霉毒素B1标准溶液质量浓度为0.591~5.91βμg/L时,峰面积与浓度呈现良好的线性关系,黄曲霉毒素B1的回收率为85.4%~98.9%（添加量分别为0.510βμg/kg、7.090βμg/kg和14.180βμg/kg）,相对标准偏差为0.2%~1.8%,方法检出限为0.1βμg/kg。运用所建立方法对市售的8个茶样及加标样品中的黄曲霉毒素B1进行检测,结果显示该方法选择性强、灵敏度高,适合茶叶中黄曲霉毒素B1的测定。
A new method for the sensitive determination of Aflatoxins B1 in tea by high performance liquid chromatography with photoelectric reactor and fluorescence detector was established. A solution of V(acetonitrile)∶V(H2O)=86∶14 was used to extract Aflatoxins B1 from tea. The extracted solution was then purified by a multifunctional and immuneaffinity column, respectively. The peak area and the concentration of Aflatoxins B1 showed a good linear relationship within the range from 0.591βμg/L to 5.91βμg/L with a linear correlation coefficient (r) of 0.9994. The recoveries at the concentrations studied [low level (7.090βμg/kg), high level (14.180βμg/kg)] were between 85.6% and 98.9% with a relative standard deviations ranging from 1.7% to 1.8%. The limit of detection (LOD) is 0.1βμg/kg (S/N=3). The limit of quantitation (LOQ) is (0.591βμg/kg). The new method was used to analyze eight tea samples collected from the local markets and negative results were obtained. The method is suitable for detection of Aflatoxins B1 in tea with high selectivity and sensitivity.
[1] Prema Viswanath, Divyashree Kallenhalli Nanjegowda, Hemalatha Govindegowda.Aflatoxin determination in black tea (Camellia sinensis)- Status and development of a protocol[J]. Journal of Food Safety, 2012, 32: 13-21.
[2] 马志科, 昝林森. 黄曲霉毒素危害、检测方法及生物降解研究进展[J]. 动物医学进展, 2009, 30(9): 91-94.
[3] 中华人民共和国卫生部. GB 2761—2011食品安全国家标准食品中真菌毒素限量[S]. 北京: 中国标准出版社, 2011: 2.
[4] GUAN Di, LI Peiwu, ZHANG Qi, et al. An ultra-sensitive monoclonal antibody-based competitive enzyme immunoassay for aflatoxin M1 in milk and infant milk products[J]. Food Chemistry, 2011, 125(4): 1359-1364.
[5] 叶雪珠, 王小骊, 赵燕申, 等. 黄曲霉毒素B1检测方法的分析[J]. 食品与发酵工业, 2003, 29(10): 90-92.
[6] 齐惠萍, 吕建明, 李常青. ELISA 法检测食醋中黄曲霉毒素B1方法的改进[J]. 中国食品卫生杂志, 2008, 20(4): 313-315.
[7] 江涛, 柳桢, 郑佳, 等. 总黄曲霉毒素ELISA定量检测方法的研制[J]. 中国食品卫生杂志, 2006, 18(4): 292-296.
[8] 赵晓娟, 冼燕萍, 罗海英, 等. 液相色谱-串联质谱法同时检测花生油中4种黄曲霉毒素[J]. 食品科学, 2011, 32(14): 194-197.
[9] NONAKA Y, SAITO K, HANIOKA N, et al. Determination of aflatoxins in food samples by automated on-line in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry[J]. Journal of Chromatography A, 2009, 1216(20): 4416-4422.
[10] TANAKA H, TAKINO M, SUGITA-KONISHI Y, et al. Development of a liquid chromatography/time-of-flight mass spectrometric method forthe simultaneous determination of trichothecenes, zearalenone and aflatoxins in food stuffs[J]. Rapid Communications in Mass Spectrometry, 2006, 20(9): 1422-1428.
[11] 朱聪英, 应永飞, 韦敏珏, 等. 液相色谱-串联质谱法测定饲料中黄曲霉毒素的研究[J]. 质谱学报, 2010, 31(4): 240-246.
[12] 付朝晖, 黄雪祥, 闵顺耕. 超高效液相色谱法快速测定发酵茶叶中的黄曲霉毒素[J]. 分析试验室, 2009, 28(6): 112-115.
浙公网安备 33019902000101号 
