中药材中氨基甲酸酯类农药的高效液相色谱-质谱分析

被引:12
作者
徐远金
李永库
机构
[1] 广西大学糖业工程技术研究中心
关键词
高效液相色谱-质谱; 固相萃取; 氨基甲酸酯农药; 中药材;
D O I
暂无
中图分类号
R284 [中药化学];
学科分类号
1008 ;
摘要
建立了高效液相色谱-质谱联用技术,分析了10种中药材中痕量氨基甲酸酯类农药残留量的方法。结合二次质谱的特征碎片离子情况初步研究了氨基甲酸酯类农药的裂解规律,样品提取液经固相萃取及C18柱分离,以不同比例的乙腈和甲酸混合液作梯度洗脱,以保留时间和质荷比对各分离组分定性,用峰面积定量。结果表明,8种氨基甲酸酯类农药的浓度与其峰面积在一定范围内呈线性关系,各农药的检出限在2.5~5.0μg·L-1之间,加标回收率在87.7%~98.4%间,相对标准偏差在2.5%~5.7%之间。仅在所分析的10种中药材的一种中测得0.043 mg·kg-1的异丙威。
引用
收藏
页码:877 / 880+884 +884
页数:5
相关论文
共 13 条
[1]  
Atrache L L E,,Sabbah S,Morizur J P.Identification of phenyl-N-methylcarbamates and their transformation products in tunisian surface water by solid-phase extraction liquid chromatography-tandem mass spec-trometry. Talanta . 2005
[2]  
Molina M,,Wiedmer S K,Jussila M, et al.Use of a partial filling technique and reverse migrating micelles in the study of N-methylcarbamate pesticides by mi-cellar electrokinetic chromatography-electrospray ionization mass spectrometry. Journal of Chromatography . 2001
[3]  
Nogueira J MF,,Sandra T,Sandra P.Considerations on ultra trace analysis of carbamates in water samples. Journal of Chromatography . 2003
[4]  
Yinon J,,Vimcze A.Collision-induced dissociation (CID) processes in some carbamate and phenylurea pesticides studied by ion-trap MS/MS. International Journal of Mass Spectrometry and Ion processes . 1997
[5]  
Bogialli S,,Curini R,Corcia A D, et al.Simple and rapid assay for analyzing residues of carbamate insecticides in bovine milk: hot water extraction followed by liquid chromatography-mass spectrometry. Journal of Chromatography . 2004
[6]  
Rosales-Conrado N,,Le‘on-Gonz‘alez M E,P‘erez-Ar-ribas L V, et al.Effect of temperature on the separation of chlorophenoxy acids and carbamates by capillary high-performance liquid chromatography and UV (or diode array) detection. Journal of Chromatography . 2005
[7]  
Zuf‘a L,,Aldaz A,Girdldez J.Simple determination of capecitabine and its metabolites by liquid chromatography with ultraviolet detection in a single injection. Journal of Chromatography . 2004
[8]  
Nakazawa H,,Takahashi N,Inoue K, et al.Rapid and simultaneous analysis of dichlorvos, malathion, carbaryl, and 2,4-dichlorophenoxy acetic acid in citrus fruit by flow-injection ion spray ionization tandem mass spectrometry. Talanta . 2004
[9]  
Ballesteros E,,Gallego M,Valcarcel M.Automatic gas chromatographic determination of N-methylcar-bamates in milk with electron capture detection. Analytical Chemistry . 1993
[10]  
Natangelo M,,Tavazzi S,Fanelli R, et al.Analysis of some pesticides in water samples using solid-phase mi-croextraction-gas Chromatography with different mass spectrometric techniques. Journal of Chromatography . 1999