| Nereistoxin insecticides are a type of compound that derived from the chemical structure of nereistoxin,which belong to animal source insecticide and can be used to control pests on crops,such as vegetables and grains.Nereistoxin insecticides have been reported about its inhibitory neurotoxicity in human and animal body,which residue in foods can cause some damage to human liver cells after being absorbed by the body,and it also can cause neuromuscular toxicity.Because of their high selectivity and high biological activity,benzoylureas are widely used in agriculture to prevent pests,which belong to insect growth regulators.The benzoylureas can kill the insects by interfering synthesis of chitin and hindering the normal growth.The residue of benzoylurea insecticides in plant may cause damage to human health through the concentration in the food chain.For example,diflubenzuron is harmful to human liver cell.Carbamate insecticides are widely used in agricultural environments to protect crops against a range of insects,which influence steroidogenesis in animals and humans.For example,carbaryl can inhibited progesterone biosynthesis of human,methomyl can cause chromosome aberrations in human and have damage to human peripheral blood lymphocytes.Organophosphorus insecticides are highly toxic,and have teratogenic and carcinogenic effects.Its residue in the food and after being absorbed by the body will cause poisoning and may cause some harm to human nervous system,especially to children's nervous system.At present,the main methods for the determination of insecticides are chromatography and chromatography-tandem mass spectrometry.In recent years,the liquid chromatography-tandem mass spectrometry(LC-MS/MS)has a good advantage for the determination of multi-component residues in food because of high sensitivity and easy operation.Therefore,it is very significant for improving the food safety system to establish the detection methods for nereistoxin,benzoylurea,carbamate and organophosphorus insecticides in foods by LC-MS/MS.In this paper,it reviews the definition,toxicity mechanism,harm,limit standards and detection methods of common nereistoxin insecticides,benzoylurea insecticides,carbamate insecticides and organophosphorus insecticides.The methods are developed to determine nereistoxin insecticides in rice flour and oatmeal,benzoylurea insecticides in the fruit and fruit products,carbamate insecticides and organophosphorus insecticides in soybean flour and fruit juice by LC-MS/MS.The results are as follows:1.The mass spectrum parameters,chromatographic conditions and pretreatment methods are optimized in the experiments.The mixed solution of acetonitrile and ethyl acetate(V:V=4:1)is used as extraction agent.Under ultrasound-assisted extraction and dispersive solid-phase extraction purification,5 kinds of nereistoxin insecticides in rice flour and oatmeal are determined simultaneously by LC-MS/MS with ESI positive or negative source under multiple reaction monitoring(MRM)segment mode.In the experiments,5mmo·L-1 ammonium acetate solution(0.1%formic)-acetonitrile(V:V=10:90)is used as mobile phase,5 kinds of nereistoxin insecticides are completely separated within 8 minutes.The good linearity of the method are achieved and the correlation coefficients(r)are above 0.9995 in the linear range of 1?100 ng·mL-1.The limits of detection(LOD)and limits of quantification(LOQ)range from 0.11 to 0.29 ?g·kg-1 and 0.37 to 0.97 ?g·kg-1,respectively.The recoveries of 5 kinds of nereistoxin insecticides in spiked sample range from 71.40%to 96.61%,the relative standard deviation(RSD)are 1.82%?6.40%.This method can be applied to detection 5 kinds of nereistoxin insecticides in real sample.2.Acetonitrile is used as extraction agent,under ultrasonic-assisted extraction and dispersive solid-phase extraction purification,a method is established for the simultaneous determination of 13 kinds of benzoylurea insecticides in fruit and fruit products by LC-MS/MS with ESI+source under MRM mode.In the experiments,0.1%formic acid aqueous solution-acetonitrile is used as the mobile phase,under gradient elution,13 kinds of benzoylurea insecticides are separated within 9 minutes.The calibration curve showed a good linear relations for 13 kinds of benzoylurea insecticides,and the correlation coefficients(r)are above 0.9995.The LOD and LOQ range from 0.03 to 0.14 ?g·kg-1 and 0.10 to 0.47?g·kg-1,respectively.The recoveries of 13 kinds of benzoylurea insecticides in spiked sample range from 78.32%to 96.92%,the RSD range from 1.48%to 6.48%.This method can be applied to detection 13 kinds of benzoylurea insecticides in real sample.3.Based on LC-MS/MS,a method is established for detecting 11 kinds of carbamates and 4 kinds of organophosphorus insecticides in soybean flour and fruit juice.Samples were extracted by acetonitrile,under ultrasonic-assisted extraction and dispersive solid-phase extraction purification.The 11 kinds of carbamate insecticides and 4 kinds of organophosphorus insecticides are separated with in 11 minutes under gradient elution with 0.1%formic acid aqeous solution-methanol as mobile phase in the experiments.The insecticides are detected by LC-MS/MS with ESI+source under MRM mode.The good linearities of the method are achieved and the correlation coefficients(r)are above 0.9996 in the linear range 0.5 to 200 ng·mL-1.The LOD and LOQ range from 0.01 to 0.14?g·kg-1 and 0.03 to 0.47 ?g·kg-1,respectively.The recoveries of the 15 Kinds of insecticides in spiked sample range from 71.21%to 99.81%,and RSD range from 1.03%to 5.28%.This method can be applied to analysis carbamate and organophosphorus insecticides in real sample. |
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