Rapid HPLC Determination of Malachite Green in Water with Solid Phase Micro-extraction
摘 要
提出了固相微萃取-高效液相色谱法测定水中孔雀石绿的含量。为使固相微萃取达到更高的效率,选择85 μm的聚丙烯酸酯(PA)涂层萃取纤维,萃取时间为15 min。以Shim-pack VP-ODS C18色谱柱为固定相分离,用pH 4.5的50 mmol·L-1乙酸铵溶液与乙腈按体积比为20比80混合的溶液为流动相进行洗脱,在波长595 nm处进行测定。孔雀石绿的质量浓度在0.05~2 mg·L-1范围内呈线性,检出限(3S/N)为0.003 mg·L-1。以鱼塘水为基体进行回收试验,方法的回收率在98.1%~109.6%之间。
Abstract
HPLC with sample treatment by solid phase micro-extraction (SPME) was applied to the determination of malachite green in water samples. To attain a higher efficiency in SPME, the 85 μm PA coating was applied to the micro-extractor, and the extraction was carried out for 15 min. The Shim-pack VP-ODS C18 column was used as the stationary phase, and a mixture of 50 mmol·L-1 ammonium acetate solution of pH 4.5 and acetonitrile (20+80) was used as the mobile phase for elution. Detection at 595 nm was adopted. Linearity range of malachite green was kept in the range of 0.05-2 mg·L-1, with detection limit (3S/N) of 0.003 mg·L-1. A sample of fish pond water was analyzed by this method, and test for recovery was made on this sample as matrix by standard addition method giving results in the range of 98.1%-109.6%.
中图分类号 O657.7
所属栏目
基金项目 浙江省自然科学基金(Y4090258);宁波市自然科学基金(2010A610191);宁波大学学科基金(xkl09071)
收稿日期 2010/9/4
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备注陶艳玲(1984-),女,湖南浏阳人,硕士研究生,主要从事食品安全分析研究。
引用该论文: TAO Yan-ling,DENG Ai-ni,LIU Qiu-mei,GUO Zhi-yong,WANG Sui. Rapid HPLC Determination of Malachite Green in Water with Solid Phase Micro-extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(9): 1092~1094
陶艳玲,邓爱妮,刘秋梅,郭智勇,王邃. 固相微萃取-高效液相色谱法快速测定水中孔雀石绿[J]. 理化检验-化学分册, 2011, 47(9): 1092~1094
被引情况:
【1】张红园,林郑忠,吴泉书,林毅东,高治昊,黄志勇, "分子印迹-固相萃取-高效液相色谱法测定鱼肉中的孔雀石绿",理化检验-化学分册 51, 390-393(2015)
【2】王金秀,任兰正, "离子液体萃取-分光光度法测定水样中的孔雀石绿",理化检验-化学分册 52, 828-830(2016)
【3】钟少枢, "高效液相色谱-串联质谱法测定多宝鱼中孔雀石绿残留量",理化检验-化学分册 52, 475-476(2016)
【4】邓婕,鲍洪波,吉洪明,吴晓清,杜诗劼, "渔业领域中孔雀石绿检测的研究进展",理化检验-化学分册 48, 1502-1507(2012)
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参考文献
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【12】杜新贞,曹旭,王雪梅,等.介孔涂层固相微萃取-高效液相色谱法测定水样中领苯二所酸酯化合物[J].分析试验室, 2009,28(8):1-4.
【2】王邃,陈丹峰,郭智勇,等.孔雀石绿的污染治理及样品中残留物的分离检测方法[J].水生态学杂志, 2009,2(4):146-150.
【3】GB/T 19857-2005水产品中孔雀石绿和结晶紫残留量的测定[S].
【4】GB/T 20361-2006水产品中孔雀石绿和结晶紫残留量的测定高效液相色谱荧光检测法[S].
【5】高华鹏,李永夫,沈维军,等.高效液相色谱-串联质谱联用测定鳗鱼中孔雀石绿、结晶紫及其代谢物残留量[J].理化检验-化学分册, 2008,44(2):103-106.
【6】龙洲雄,万春花,胡海山,等.高效液相色谱快速测定水产品中孔雀石绿、结晶紫及其无色产物的残留量[J].理化检验-化学分册, 2010,46(4):368-373.
【7】任秀莲,魏琦峰,程春萍,等.高效液相色谱测定水产品中孔雀石绿、结晶紫及其代谢物残留量的研究进展[J].中国卫生检验杂志, 2007,17(1):173-173.
【8】ZHANG Zhou-yao, YANG Min-jun, PAWLISZYN J. Solid-phase microextraction. A solvent-free alternative for sample preparation[J]. Anal Chem, 1994,66(17):844-853.
【9】杨宇川,辉永庆,何小波,等.固相微萃取法的纤维涂层的研究进展[J].理化检验-化学分册, 2008,44(9):904-910.
【10】AI J. Solid phase microextraction for quantitative analysis in nonequilibrium situations[J]. Anal Chem, 1997,69(6):1230-1236.
【11】HERNANDEZ F, BELTRAN J, LOPEZ F J, et al. Use of solid-phase microextraction for the quantitative determination of herbicides in soil and water samples[J]. Anal Chem, 2000,72(10):2313-2322.
【12】杜新贞,曹旭,王雪梅,等.介孔涂层固相微萃取-高效液相色谱法测定水样中领苯二所酸酯化合物[J].分析试验室, 2009,28(8):1-4.
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