Simultaneous determination of carbamate pesticide residues in purple yam by high performance liquid chromatography-tandem mass spectrometry
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摘要: 通过超高液相色谱-串联质谱联用（LC-MS/MS）技术,建立了一种高灵敏度检测紫薯蓣中农药残留的方法。样品经环己烷-乙酸乙酯（1∶1,V/V）提取,全自动凝胶净化在线浓缩仪净化,然后采用LC-ESI（+）-MS/MS测定,对液质分离条件进行优化。实验结果表明,5种氨基甲酸酯农药在1.050.0μg/L范围内线性关系良好,相关系数0.99830.9999;在2.010.0μg/kg浓度范围内,加样回收率82.05%97.27%之间,相对标准偏差2.85%6.63%。该方法具有快速、准确、简便、灵敏、净化效果好、人为误差小的特点。
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关键词:
- 紫薯蓣 /
- 氨基甲酸酯类农药 /
- 快速高分离液质联用技术
Abstract: The high sensitive liquid chromatography-tandem mass spectrometry ( LC-MS/MS) had been developed for the detection of 5 carbamate pesticides in purple yam.After extraction of the pesticides with cyclohexane and ethyl acetate ( v /v = 1∶1) , the extract was purified by automatic gel purification system using cyclohexane and ethyl acetate ( v /v = 1 ∶ 1) as mobile phase.Analysis was performed by liquid chromatography- electrospray ionization-tandem mass spectrometry operated in the multiple reaction monitoring ( MRM) mode, and the separation conditions were optimized.The results showed that calibration curves were linear and covered from 1.0 to 50.0μg /L, and the correlation coefficients was 0.99830.9999.The average recoveries, measured at 2.0 to 10.0μg /kg, were in the range82.05% to 97.27% for all of the compounds tested with relative standard deviations were between 2.85% to 6.63%.The results indicated that the method had been demonstrated to be simple, accurate, practical and high sensitive for the determination of carbamates residues in purple yam samples. -
[1] Tewtrakul S, Itharat A.Anti-allergic substances from the rhizomes of Dioscorea membranacea[J].Bioorganic Medicinal Chemistry, 2006, 14 (24) :8707-8711.
[2] Kelmanson J E, Jager A K, Van Staden J.Zulu medicinal plants with antibacterial activity[J].Journal of Ethnoparmacology, 2000, 69 (3) :241-246.
[3] Chen Y T, Kao W T, Lin K W.Effects of pH on the total phenolic compound, antioxidative ability and the stability of dioscorin of various yam cultivars[J].Food Chemistry, 2008, 107 (1) :250-257.
[4] Miyazawa M, Shimamura H, Nakamura S, et al.Antimutagenic activity of (+) -β-eudesmol and paeonol from dioscorea japonica[J].Journal of Agricultural and Food Chemistry, 1996, 44 (7) :1647-1650.
[5] 唐柏彬, 郗存显, 邹芸, 等.液相色谱法同时测定火锅底料中11种氨基甲酸酯类农药残留[J].食品科学, 2013, 34 (10) :191-196. [6] 邓立刚, 李增梅, 郭长英, 等.超高效液相色谱-串联质谱法测定蔬菜中7种氨基甲酸酯类农药残留[J].食品科学, 2011, 32 (6) :221-224. [7] 孙涛, 刘河疆, 胡开峰, 等.超高效液相色谱-串联质谱法快速测定蔬菜中7种氨基甲酸酯类农药残留[J].分析实验室, 2010, 29 (4) :87-91. [8] 林诗云, 吴晓波, 陈海云, 等.固相萃取-高效液相色谱法测定水中6种氨基甲酸酯类农药残留量[J].农药, 2010, 49 (12) :909-910. [9] The Compilation of Residue Lim its Standard s for Pseticides and Veterinary Drugs in Food stuffs in Major Trading Countries and Reigons.Beijing:China Standards Press, 2004.
[10] Moreno-González D, Huertas-Pérez J F, García-Campaa A M, et al.Ultrasound-assisted surfactant-enhanced emulsification microextraction for the determination of carbamates in wines by ultra-high performance liquid chromatographytandem mass spectrometry[J].Journal of Chromatography A, 2013, 1315:1-7.
[11] Fernández M, PicóY, Maes J.Determination of carbamate residues in fruits and vegetables by matrix solid-phase dispersion and liquid chromatography-mass spectrometry[J].Journal of Chromatography A, 2013, 871 (1-2) :43-56.
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