生鲜乳中兽药残留的快速筛查与风险预警体系构建

Rapid screening and early risk assessment of veterinary drug residues in raw milk

该研究探索并构建一种基于历史数据分析的安全预警方法,对生鲜乳中兽药残留情况进行识别、控制与评价,以便在风险发生之前做出准确判断。首先利用高效液相色谱-高分辨飞行时间串联质谱(High Performance Liquid Chromatography-high Resolution Time-of-flight Tandem Mass Spectrometry,HPLC-TOF-MS/MS)方法对上海市各牧场的生鲜乳进行兽药残留筛查,然后以生鲜乳中泼尼松(Prednisone,Pre)残留检出数为例,利用休哈特控制图(Shewhart control charts)构建风险预警体系。结果表明:在300个生鲜乳样品中共筛查出42种兽药残留,涉及类固醇类(12种)、糖皮质类(6种)和镇静剂(5种)等12大类;在筛查的6个星期中,泼尼松检出数(Number of Prednisone Detected,Pn)控制图呈现稳定的状态;当假设第7周泼尼松检出数为6时,Pn控制图呈现稳态,未触发预警;当假设第7周泼尼松检出数为10时,Pn控制图出现异常,稳态遭到破坏,此时该批样品触发风险预警。综上,利用HPLC-TOF-MS/MS能对生鲜乳样品进行高通量的兽药残留筛查,再利用休哈特控制图结合历史数据可以对生鲜乳样品的兽药残留进行有效的风险监测和预警。

The production of raw milk is a dynamic and continuous process.There can be some new changes in the quality of produced raw milk every day.A delay determination can occur in the product safety system when assessing veterinary drug residues in the subsequent procedure using the current detection data.The purpose of this study aims to construct an early warning system based on the full-scale historical data,which can be used to identify,control and evaluate veterinary drug residues in raw milk,and then make accurate judgments before risks occur.Three parts include in this system.1)The raw milk samples from 50 pasture in Shanghai were first taken as the population to be sampled based on statistical principles.The population was divided into different parts in each pasture.The simple random sampling method means to take samples from various parts,and combine them to obtain the final screening sample.Specifically,the fresh milk samples from 50 pasture in Shanghai were taken once a week,and a total of 300 screening samples were obtained for 6 weeks in May and June.The screening results of veterinary drug residues in these raw milk samples indicated the contamination conditions of veterinary drugs during the sampling period.2)The collected samples were then tested.The detection test was performed on the high performance liquid chromatography,high resolution time-of-flight tandem mass spectrometry(HPLC-TOF-MS/MS)by mixing standard working solutions.A total of steroidal veterinary drugs(12 types),glucocorticoids(6 types),sedatives and quinolones(5 types each)were detected in this study.There were 42 types of veterinary drug residues in total associated with 12 categories of veterinary drugs.Six veterinary drugs were detected in every batch:Thiabendazole,Altrenogest,Beclomethasone,Carazolol,Methyltesterone,and Norethandrolon,indicating the contamination of the veterinary drug in these pastures.3)A risk warning system was finally constructed.When the number of collected samples was fixed for the screening of the veterinary drug residues in raw milk for each batch from the pastures,the number of prednisone detected(Pn)control chart can be chosen to establish a risk early warning system based on the results of screening of veterinary drug residues.During the 6-week screening,the Pn control chart showed a stable state.When the number of detected prednisone was 6 in the 7th week,it infers that the Pn control chart still showed a stable state.When the prednisone detection number was 10 in the 7th week,the Pn control chart was abnormal in the unsteady state,indicating the batch of samples triggered the warning.All the results show that the established risk warning system can be real-time monitor.This proposed system can play an early warning and preventive role in the occurrence of safety risks for the veterinary drug residues in raw milk.