摘要
通过对干燥剂、分散吸附剂的种类及质量进行对比及优化,对鲮体内孔雀石绿（MG）及其代谢物的分散固相萃取/高效液相色谱-串联质谱（Qu ECh ERS-HPLC-MS/MS）联用方法进行了优化。方法以乙腈为萃取溶剂,无水硫酸镁为干燥剂,乙二胺-N-丙基硅烷（PSA）与石墨化炭黑（GCB）为分散吸附剂,电喷雾正离子模式（ESI＋）,多反应监测模式,内标法定量。结果显示,无水硫酸镁对样品中水分干燥效果良好,50 mg PSA＋10 mg GCB可达到净化效果。在优化条件下,MG和无色孔雀石绿（LMG）在1-50 ng/m L范围内呈现良好的线性相关,相关系数r分别为0.999 21和0.999 37;方法检测限（LOD,S/N=3）为0.5μg/kg。采用该方法对鲮空白样品进行检测及加标回收率的测定,在2.0、10、25μg/kg 3个浓度水平下,MG的加标回收率为82.5%-92.6%,LMG的加标回收率为84.6%-95.1%。将该方法用于鲮体内MG及LMG残留消除规律研究,得到MG和LMG的消除半衰期分别为13.6、178.3 h,表明MG在鲮体内消除相对较快,但是其主要代谢产物LMG消除缓慢,直到40 d后低于检测限。本研究可为鲮等水产品中MG和LMG的检测提供支持技术,为水产品质量安全监管提供参考数据。
QuEChERS （quick, easy, cheap, effective, rugged and safe） extraction and high performance liquid chro- matography tandem mass spectrometry （QuEChERS- HPLC -MS/MS） were optimized by comparing and optimizing desiccants and adsorbents for determination of malachite green （MG） and its primary metabolite （ i. e. leuco - mala- chite green, LMG） in mud carp （Cirrhina molitorella） in the study. The extraction method of mud carp tissues adopt- ed acetonitrile as extractants, anhydrous magnesium sulfate as a desiccant, and the mixture of primary secondary a- mine （PSA, 50 rag） and graphitized carbon blacks （GCB, 10 mg） as adsorbents. The identification of malachite green （MG） and leuco- malachite green （LMG） was achieved by using electrospray ionization in positive ion mode （ ESI ＋ ） under multiple reaction monitoring mode. The quantitative analysis of MG and LMG was performed by the in- ternal standard method. Under the optimized condition, MG and LMG showed a good linearity in their concentration range of 1 - 50 ng/mL with the correlation coefficient of 0. 998 77 and 0. 997 32, respectively. Both of their detection limits（ LOD, SIN = 3 ） were 0.5 μg,/kg. The recoveries of MG and LMG at three spiked levels of 2, 10 and 25 μg/kg were ranged of 82.5% -92.6% and 84.6% -95.1% respectively. By applying the proposed method to study the residues and elimination rules of malachite green and its primary metabolite in mud carp, results showed that the elim- ination half life of MG and LMG were 13.6 and 178.3 h, respectively. It suggested that MG was depleted relative fas- ter in mud carp. In contrast, the elimination of LMG, as the main metabolite of MG, was slower, and the content of LMG was below the detection limit until 40 d. The study would provide technical supports for detection of MG and LMG and reference data for quality safety of aquatic products.
作者
刘书贵
尹怡
李丽春
单奇
朱新平
马丽莎
戴晓欣
郑光明
LIU Shugui YIN Yi LI Lichun SHAN Qi ZHU Xinping MA Lisha DAI Xiaoxin ZHENG Guangming(Ministry of Agriculture/Ministry of Agriculture Laboratory of Quality ＆ Safety Risk Assessment for Aquatic Product （ Guangzhou Key Laboratory of Tropical ＆ Subtropical Fishery Resource Application ＆ Cultivation, Pearl River Fisheries Institute, Chinese Academy of Fishery Sciences, Guangzhou 510380,China)
出处
《中国渔业质量与标准》
2016年第5期45-51,共7页
Chinese Fishery Quality and Standards
基金
水产品养殖禁限用药物调查与产品安全性评估(GJFP201501001)
广东省质量安全专项项目
