对渔用中药制剂中违法添加西药成分的快速筛查与确证  

Rapid screening and confirmation of western medicine adulteration in Chinese herbal medicines for fishery

作　　者：严华[1] 刘鑫[1] 张海燕[2] 崔凤云[1] 李建辉[1] 云环[1] 丁双阳[3] 张朝晖[1] 杨大进 

机构地区：[1]北京出入境检验检疫局检验检疫技术中心食品实验室,北京100026 [2]温州医学院,温州325000 [3]中国农业大学动物医学院,北京100193 [4]国家食品安全风险评估中心,北京100021

出　　处：《中国食品卫生杂志》2013年第5期391-396,共6页Chinese Journal of Food Hygiene

基　　金：科技部质检公益行业科研专项(201210029);国家高技术研究发展计划(863计划)(2012AA101603)

摘　　要：目的采用超高效液相色谱-线性离子阱轨道离子阱组合式高分辨质谱联用技术(UPLC-LTQ Orbitrap MS),建立渔用中药制剂中氟喹诺酮类、磺胺类、四环素类、孔雀石绿类、硝基呋喃类以及喹噁啉类等48种西药成分的快速筛查与确证方法。方法样品经乙酸乙酯提取,C18吸附剂净化,经反相色谱柱分离,甲醇-水(含0.1%甲酸)为流动相梯度洗脱(流速250μl/min,柱温30℃,进样量10μl),通过LTQ Orbitrap MS全扫描,TOXID软件结合数据库检索,对48种西药成分进行快速筛查和确证。结果各化合物的检出限(LOD)为0.006 0～0.21 mg/kg;定量限(LOQ)为0.020～0.72 mg/kg,在线性范围内存在良好线性关系,相关系数r2为0.9796～0.9997;在0.25、0.50、1.00 mg/kg三个添加水平下,方法回收率分别为81.9%～114.4%、84.0%～114.3%、80.9%～114.8%,RSD为1.56%～14.3%。结论方法快速、准确、可靠、重现性好,可对中药基质中的部分违法添加药物进行筛查和确证。Objective To develop a screening and confirmation method of UPLC-LTQ Orbitrap MS for 48 chemical medicine including fluoroquinolone, sulfanilamide, tetracycline, malachite green, nitrofuran, olaquindox and carbadox mixed into traditional Chinese herbal medicine for fishery. Methods The samples were extracted by ethyl acetate, cleaned by Cls sorbent, separated by reversed phase chromatography （Velocity： 250μl/min, Cylinder temperature： 30 ℃ , Sample size： 10 μl） , and gradient eluted with methanol/water （containing 0. 1% formic acid）. Final detection was performed by LTQ Orbitrap MS in full scanning mode. The TOXID software combined with database retrieval was used for screening and confirmation of 48 veterinary drugs. Results The limits of detection （LODs） and the limits of quantification （LOQs） of 48 veterinary drugs were 0. 006 0 -0.21 mg/kg and 0. 020 -0.72 mg/kg, respectively. The method showed good linearity over the linear range, r2 = 0. 9796 -0. 9997. The recoveries were 81.9% - 114.4% , 84.0% - 114. 3% , 80.9% - 114. 8% for the three spiked levels at 0.25, 0.50 and 1.0 mg/kg, respectively. The RSDs were in the range of 1.56% - 14.3%. Conclusion The method was rapid, accurate, reliable and precise. It was suitable for the screening and confirmation of chemical medicine adulterated into traditional Chinese herbal medicine.

关 键 词：超高效液相色谱 高分辨质谱 渔用中药制剂 筛查 违法添加物 食品安全 

分 类 号：R155.5[医药卫生—营养与食品卫生学]