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。
Eight carbamate residues in 10 varieties of Chinese herbal medicines were determined by HPLC-MS with preliminary separation by solid-phase extraction. The fragmentation pattern of carbamate pesticides were studied preliminarily. Acetonitrile extract of the sample was separated on ODS C18 column, and the pesticides were eluted with methanol. The eluate was evaporated nearly to dryness, and made up to 1.0 mL with the mobile phase solution. Further separation was made on XDB C18 column, by gradient elution with mobile phase of mixed solutions with diffent ratio of CH3CN and HCOOH solutions. The earbamate pesticides were identified by retention time and m/z ratio, and determined by peak area. Linearity of concentration of 8 carbamate pesticides with their peak area were obtained with detection limits between 2. 5-5. 0 μg · L^-1. RSD's obtained were between 2. 5%-5. 7% and recoveries in the range of 87.7%-98. 4%. Pesticide of O. 043 mg·kg^-1 of isoprocarb was found in only one of the 10 samples of Chinese herbal medicine analyzed.
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2006年第11期877-880,884,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
广西自然科学基金(0009010)
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
HPLC-MS
Solid phase extractiom Residual earbamate pesticides
Chinese herbal medicine