HPLC-MS/MS Determination of Residual Amount of Bensultap in Vegetables
摘 要
采用高效液相色谱-串联质谱法测定蔬菜中杀虫磺的残留量。称取样品的匀浆10.00 g,用乙腈提取3次(每次20 mL),合并提取液并将其蒸缩至约5 mL。此溶液通过TPT固相萃取柱净化,保留流出液(主液)。用乙腈-甲苯(3+1)混合液25 mL淋洗固相萃取柱,淋出液与主液合并,先在45℃水浴浓缩至约5 mL,再于35℃水浴上吹氮蒸干。用甲酸-乙腈(0.1+99.9)混合液溶解残渣并定容至10 mL。按所选条件进行高效液相色谱-串联质谱法分析。杀虫磺的质量浓度在1~500 μg·L-1内与其对应的峰面积呈线性关系,不同基质中杀虫磺的检出限(3S/N)为0.1~0.4 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为48.0%~97.7%,测定值的相对标准偏差(n=6)为1.8%~12%。
Abstract
HPLC-MS/MS was applied to the determination of residual amount of bensultap in vegetables. Homogenized pulp (10.00 g) of the sample was taken and extracted thrice with CH3CN (20 mL each). The combined extract was evaporated to about 5 mL. The solution was then purified by passing through TPT SPE column. The eluate (main) was reserved. The SPE column was rinsed with 25 mL of a mixture of CH3CN and toluene (3+1). The eluate was combined with the main eluate, and evaporated first to about 5 mL at 45℃ in a water bath and then to dryness by N2-blowing at 35℃ in the water bath. The residue was taken up and made up to 10 mL with a mixture of formic acid-CH3CN (0.1+99.9). The solution was then analyzed by HPLC-MS/MS under the condition described. Linear relationship between values of peak area and mass concentration of bensultap was kept in the range of 1-500 μg·L-1, with detection limit (3S/N) of bensultap in different matrixes in the range of 0.1-0.4 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method. Values of recovery found were in the range of 48.0%-97.7%, with RSD's (n=6) in the range of 1.8%-12%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201802014
所属栏目 工作简报
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收稿日期 2017/2/24
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备注陈俊(1972-),男,四川德阳人,工程师,主要从事色谱在食品检验中的应用工作,chenjunxiansheng@163.com
引用该论文: CHEN Jun,GOU Jian,LIAO Min,CHEN Hong. HPLC-MS/MS Determination of Residual Amount of Bensultap in Vegetables[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(2): 192~195
陈俊,苟健,廖敏,陈红. 高效液相色谱-串联质谱法测定蔬菜中杀虫磺的残留量[J]. 理化检验-化学分册, 2018, 54(2): 192~195
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【6】王银淑,张春造,韩嘉祥,等.高效低毒新型杀虫剂-杀虫磺防治水稻害虫的试验研究[J].华北农学报, 1986(4):73-78.
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【8】韩招久,韩召军,姜志宽,等.沙蚕毒素类杀虫剂的毒理学研究新进展[J].现代农药, 2004,3(6):5-8.
【9】杨玲英.浅析使用"沙蚕毒素类"农药对饲养家蚕的危害及对策[J].上海农业科技, 2010(5):79-79.
【10】景成,宋俊荣.家蚕农药中毒的发生与防治[J].江苏蚕业, 2007(1):13-17.
【11】宋庆银,陈宏仁.沙蚕毒素对桑叶的污染及防范措施[J].江苏蚕业, 1993(2):24-25.
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【13】INOUE M, YAMAMOTO A. An analytical method of bensultap residues in crops and soils[J]. Journal of Pesticide Science, 1986,11(4):547-555.
【14】黄志强.食品中农药残留检测指南[M].北京:中国标准出版社, 2011.
【15】施天益.高效液相色谱法测定杀虫磺含量[J].农药, 1989,28(2):16-16.
【16】许文娟,王振刚,丁葵英,等.QuEChERS/液相色谱-串联质谱法测定5种蔬菜中17种氨基甲酸酯类农药的基质效应研究[J].分析测试学报, 2017,36(1):54-60.
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