| Veterinary antiparasite drugs is a kind of common medicine which can kill or/and remove parasite in animal vivo and vitro. According to the pharmacological effects, Veterinary antiparasite drugs can be divided into antinematodal drug, antitrematode drug, anticestodal drug, antiprotozoal drug and antiectoparasite drug, and so on. Veterinary antiparasite drugs play a good role on kill or/and remove parasite. However, the antiparasite residues bring a threat to food safety. Veterinary antiparasites drugs residue can be directly on human to produce the acute and chronic toxicity effect, and cause the parasitic resistance increase. It also can cause potential hazard to human health through the indirect effect of the environment and the food chain. From a long term view, veterinary antiparasites drug residue will affect the development of animal husbandry and aquaculture in China and to go into the international market. So, many countries and regions include China set the maximum residue limits (MRLs) for a variety of antiparasite drug in tissues, milk and eggs, and some drugs were banned to use. Therefore, residual analysis research and detection method developping, strengthen veterinary drug residue monitoring in animal-derived food, are very important steps in the food safety control. For monitoring of contaminants and veterinary drugs in food items, fast and simple and high throughput and high efficiency are becoming development tendency. Generally an analytical strategy is recommended using a two-step approach:a screening method, with a high sample throughput and an acceptable percentage of false positive results; And, a confirmation method, to confirm any positive results from the screening thereby preventing false positive results. However, there is rarely screening method for antiparasites drug residues detection is reported in resently. For the reported quantitative confirmatory method, which only involved less than fourty parasites drugs and only included the liver, milk and other single type of matrix, it is not comprehensive. Therefore, conforming to the residue analysis development trend of high throughput and high efficiency, a screening method have been developped for the quantitation screening of128veterinary antiparasite drug residues in animal-derived food. The QuEChERS sample preparation technology have been used, which can save sample preparation time and improve monitoring analysis efficiency. The study will provide technical support and theoretical basis for veterinary antiparasite drugs residue monitoring, enrich the residue monitoring system the animal-derived food, and also provide guidance and reference for animal-derived food safety evaluation.A multi-residue sreeening method for the detection of128veterinary antiparasite drugs in animal tissues (fish, muscle and liver and kidney form chicken, porcine and bovine), milk, egg, honey was developed using a QuEChERS sample preparation technology and a High-pressure liquid chromatography-electrospray ionisation-coupled to tandem mass spectrometry (HPLC-MS/MS). The modified QuEChERS technology has been used to sample preparation. The procedure consisted of a acetonitrile and ethyl acetate two repeated extraction; and then a D-SPE clean-up step, with ODS sorbent and anhydrous magnesium sulfate which choose from several common sorbent based on the ability of adsorb impurities and drugs; and then a evaporation step under a stream of nitrogen at40℃the residue was analysed by HPLC-MS/MS. A reversed phase C18analytical column was selected for chromatographic separation of the drugs in sample. Elution solvents used12.5mM ammonium formate aqueous (A) and12.5mM ammonium formate-methanol:acetonitrile (50:50, v:v)(B) with gradient elution, to make sure that the retention time of all drugs can be separated in40min. The drugs were identified using TSQ-MS in MRM mode with swiching between positive and negative scan mode in the optimal mass spectrum parameters. The analytical method was validated according to the EU guidelines (2002/657/EC) for a quantitative screening method. The LOD and LOQ was0.5-10μg/Kg and1-20μg/Kg for all drugs in the animal tissues and products; For98%of the compounds which have MRLs, the CCβ are within2times the VL; For60%of the compounds which no MRLs, the CC(3are within3times the VL. The method is adequate sensitivity to detect drugs at the concentrations below the MRLs. The results for repeatability (%RSD<26%) and the accuracy (recovery was between29.6%-83.6%) were satisfactory. The method is accurate enough to differentiate between suspected and negative sample. The result show that the method this study developped is conform to the requirements of2002-657-EC about quantitative screening method, and can meet the residue monitoring requirements.This research first developped a multi-residue sreeening method for the detection of veterinary antiparasite drugs in muscle, liver, kidney form chicken, porcine and bovine, fish milk, egg, honey by HPLC-MS/MS using a QuEChERS sample preparation technology. More sample and drugs were covered in this method, reached the high throughput requirement of screening method; And using the QuEChERS sample extraction and purification system which can save analysis time and cost; has obvious advantages on residual screening of a large number of samples. It is fullfill the gaps in this field, enrich the residue monitoring system in animal-derived food. |
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