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浙江大学学报（农业与生命科学版）
浙江大学学报(农业与生命科学版)  2014, Vol. 40 Issue (3): 330-    DOI: 10.3785/j.issn.1008-9209.2013.09.061
资源与环境科学     
超高效液相色谱串联质谱法测定环境底泥中的孔雀石绿
梅光明, 郭远明, 张小军, 严忠雍, 李佩佩, 尤炬炬, 丁跃平*
（浙江省海洋水产研究所浙江省海水增养殖重点实验室,浙江 舟山316021）
Determination of malachite green in sediment by ultra performance liquid chromatography-mass spectrometry
Mei Guangming, Guo Yuanming, Zhang Xiaojun, Yan Zhongyong, Li Peipei, You Juju, Ding Yueping*
(Key Lab of Mariculture and Enhancement of Zhejiang Province, Marine Fishery Research Institute of Zhejiang Province, Zhoushan, Zhejiang  316021,China
)
 
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摘要： 建立以多壁碳纳米管为固相萃取吸附剂分离净化水产养殖环境底泥中的孔雀石绿(malachite green,MG)和隐色孔雀石绿(leucomalachite green,LMG),并用超高效液相色谱串联质谱仪(UPLC-MS/MS)测定方法,考察不同类型固相萃取小柱、多壁碳纳米管填料孔径大小及用量、洗脱剂的种类和体积对萃取效果的影响,优化固相萃取条件。在优化试验条件下,方法的线性范围为0.05~10.0 μg/L,相关系数(r)大于0.995, MG和LMG的方法检出限分别为0.03和0.07 μg/kg,定量限分别为0.10和0.20 μg/kg。对空白底泥样品分别进行0.50，2.00，5.00 μg/kg 3种水平下的加标回收试验,MG加标回收率为97.1%~108.3%,LMG加标回收率为94.7%~110.5%,测定的相对标准偏差(relative standard deviation,RSD)均小于8.3%。该方法简单快速,前处理成本低,灵敏度高,重现性好,回收率高,可用于水产养殖环境底泥中孔雀石绿的测定。  
Abstract: Malachite green (MG) is a kind of triphenylmethanedyes, which had ever been widely used around the world as fungicide, ectoparasiticide and antiseptic in the aquaculture. Current datas  suggest that both MG and its metabolite leucomalachite green (LMG) may be carcinogenic and mutagenic. For those reasons MG has been banned in aquaculture industry in European Commission and U.S.A, and is also not approved in China. However, owing to low cost and marked effect, MG may still be used illegally. Additionally, the environment has been polluted because of MG’s wide use before. Much of the pollutants have been transferred to sediment. In order to guarantee the safety of aquaculture, a sensitive and selective analytical method is needed for the determination of MG in aquaculture sediment. The current researches  mainly focus on the determination of MG in aquatic products, rarely in sediment. Due to the matrix complex of sediment, sample pretreatment technology is the key technology. As a new type of functional material, muti-walled nanotubes (MWCNTs) have extensive prospect in the field of analytical chemistry. Now several articles have illustrated that MWCNTs have been used in the pretreatment of heavy metals and organic pollutants. Few literatures available were involved in determination of MG in sediment. During the past research, much more expensive materials such as cation exchange columns or alumina columns were mostly applied as solid-phase extraction adsorbents to determine MG in aquatic products and water. However, with advantages of lower price and good chemical properties, MWCNTs still have not been well used in analysis of MG. Now, a method for the determination of MG in sediment was established by using MWCNTs as solid-phase extraction adsorbents combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sediment sample was extracted by acetonitrile and cleaned up on MWCNTs  solid phase extraction (SPE) cartridges. The effects of experimental conditions, including SPE cartridge type, diameter and loading amounts of MWCNTs, as well as type and volume of the eluent on the extraction efficiency were investigated. Chromatographic separation was carried out on UPLC C18 column (2.1 mm×50 mm, 1.7 μm). The mass spectrometer was performed using multiple reaction monitoring (MRM) with electrospray ionization in positive mode. Under the optimized conditions, the analytes were in good linearity in the range of 0.0510.0 μg/L with the correlation coefficients (r) all above 0.995. The limits of detection were 0.03, 0.07 μg/kg for MG and LMG, and limits of quantity were 0.10, 0.20 μg/kg, respectively. Spiked at three concentration levels of 0.50, 2.00 and 5.00 μg/kg, the recovery rates of MG, LMG were 97.1%108.3% and 94.7%110.5% and the relative standard deviations (RSD) were all within 8.3%. In conclusion, MWCNTs have good performance in the enrichment and purification. The proposed method has advantages of good reproducibility, high recovery, simplicity, and low cost, and can be successfully applied for the determination of malachite green in aquaculture sediment.  
出版日期: 2014-05-20
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梅光明
郭远明
张小军
严忠雍
李佩佩
尤炬炬
丁跃平*

引用本文:

梅光明, 郭远明, 张小军, 严忠雍, 李佩佩, 尤炬炬, 丁跃平*. 超高效液相色谱串联质谱法测定环境底泥中的孔雀石绿[J]. 浙江大学学报(农业与生命科学版), 2014, 40(3): 330-.

Mei Guangming, Guo Yuanming, Zhang Xiaojun, Yan Zhongyong, Li Peipei, You Juju, Ding Yueping*. Determination of malachite green in sediment by ultra performance liquid chromatography-mass spectrometry. Journal of Zhejiang University (Agriculture and Life Sciences), 2014, 40(3): 330-.

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http://www.zjujournals.com/agr/CN/10.3785/j.issn.1008-9209.2013.09.061    或    http://www.zjujournals.com/agr/CN/Y2014/V40/I3/330

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