Determination Of Phenothiazine Sedatives,Neonicotinoid Pesticides And Acetanilide Herbicides In Food By Liquid Chromatography Tandem Mass Spectrometry

Chlorpromazine and promethazine of phenothiazine sedatives, not only can reduce the mortality rate of animals in transportation, but also has fertility effect. The wintermine composed of chlorpromazine and promethazine has the effects of antiemetic, anti-dizziness, motion sickness and sedative hypnotic. The metabolic residues of chlorpromazine and promethazine can cause leucopenia and agranulocytosis, which can result in the liver, kidney disease, and eye complications in human. Although neonicotinoid insecticides is widely used in the world, the research show that the neonicotinoid insecticides have an adverse effect on pollinating insects and birds, low toxicity to mammals, and potential threat to human health through the food chain enrichment. Thus, the application of neonicotinoid pesticides are very concerned in the worldwide, some countries restrict or even prohibit the use of neonicotinoid pesticides. Acetanilide herbicides are the most widely used herbicides, the recent studies have shown that acetanilide herbicides can be degraded to dialkylquinoneimine, which has carcinogenicity and increases the risk of cancer in animals. Additionally, acetanilide herbicides and their metabolites can cause lymphocyte sister chromatid exchange. Therefore, it is very significant for improving the food safety to establish the testing methods for phenothiazine tranquilizers in food of animal origin, neonicotinoid and acetanilide herbicides in food of plant origin. Liquid chromatography tandem mass spectrometry(LC-MS/MS) has the characteristic of high sensitivity and accuracy, so it has been used widely in the field of food safety testing.In this paper, it reviews the physical and chemical properties, toxicity mechanism and harm, limited standards and testing methods for common phenothiazine sedatives, neonicotinoid insecticides, and acetanilide herbicides. In addition, through dispersive solid phase extraction or solid phase extraction, LC-MS/MS methods are developed to determine phenothiazine sedatives in poultry eggs, neonicotinoid pesticides in infant food and acetanilide herbicides in the fruit and fruit products.The results are as follows:In this section, the optimal mass spectrum parameters and chromatographic conditions are chosen by the optimization of the mass spectrometry and chromatography conditions. Through optimization of pretreatment method, the acetonitrile is used as protein precipitation and extraction agent. Under ultrasound-assisted extraction and dispersive solid phase extraction purification, 2 kinds of phenothiazine sedatives in poultry eggs are determined by LC-MS/MS with ESI+ source and multiple reaction monitoring(MRM) mode. Using 0.1% formic acid aqueous solution- acetonitrile(V: V = 35: 65) as the mobile phase, promethazine and chlorpromazine can be completely separated within 4 minutes. The correlation coefficient(r) is above 0.999 within their respective linear ranges. And the limit of detection(LOD) for promethazine and chlorpromazine are 0.05 μg/kg and 0.10 μg/kg, The limit of quantification(LOQ) are 0.17 μg/kg and 0.23 μg/kg, respectively. The spiked recoveries of promethazine and chlorpromazine range from 80.23% to 102.02%, and relative standard devitation(RSD) are 1.92%-8.07%.2. The mixed solution of acetonitrile and ethyl acetate(V:V= 4:1) is used as extraction agent. After ultrasonic assisted extraction and the dispersive solid-phase extraction, 8 kinds of neonicotinoid pesticides are determined in infant food by LC-MS/MS with ESI+ source and MRM mode. Within 7 minutes, 8 kinds of neonicotinoid pesticides can be separated under gradient elution. Good linear relations are obtained with r >0.999, and the LOD and LOQ range from 0.02 to 6.20 μg/kg and 0.07 to 20.67 μg/kg, respectively. The spiked recoveries of 8 kinds of neonicotinoid pesticides range from 62.47% to 104.76%, and the RSD are from 1.16% to 8.70%.3. The mass spectrum parameters, chromatographic conditions and pretreatment method are optimized. Using petroleum ether(30~60℃) as extraction agent, through auxiliary oscillation extraction and Florisil PR solid-phase extraction column purification,10 kinds of acetanilide herbicides are determined in fruits and fruit products by LC-MS/MS with ESI+ source under MRM mode. Under gradient elution, 10 kinds of acetanilide herbicides can be separated within 11 minutes. The good linearity are achieved with r >0.999. And the LOD and LOQ range from 0.05 to 4.15 μg/kg and 0.17 to 13.83 μg/kg, respectively. The spiked recoveries of 10 kinds of acetanilide herbicides range from 79.15% to 99.16% with RSD of 1.86%- 8.83%.