LabChallenges实验室挑战概要.ppt

Picture – Bad ? It DOES matter Data Acceptability Methodology 方法 Equipment 设备 Procedures运行程序 Data Generation 数据生成 Enforcement methods Certified Equipment Enforcement Methods Method Improvements 方法改进 Major modifications方法大改 Minor changes方法小改 Independent Laboratory Validation 独立实验室方法验证 Funding from USDA NIFA Michigan State University Acknowledgements * * * Challenges in GLP Analytical Laboratory残留GLP实验室面临的挑战 Wayne Jiang, PhD Michigan State University Outline Introduction 介绍 Labs/Methods 实验室/方法 Challenges 挑战? Acknowledgements 致谢 IR-4 Project Since 1963 IR-4 has been a US government funded research program to facilitate registration of sustainable pest management technology for specialty crops and minor uses What is IR-4? 美国 农药登记 小宗作物 IR-4 Program-Partnerships What is IR-4? 美国农业部农业食品研局* 美国环保局美国农科院*大学*农药公司 农产品种植食品加工消费者 Sample Prep 化学 (不变) Detector Chromatogram Start Injection Response Time Injector Column He Vent Gas Chromatograph 分析仪器 (改进) HPLC Injector Detector Column Solvents Pumps Mixer Chromatogram Start Injection Response Time Waste 分析仪器 (提高) Detectors Flame Ionization Detector (FID) Selective Detectors (NPD) Photo Ionization Detector (PID) Electron Capture Detector (ECD) Mass Spec Detector (MSD MS/MS) UV Detector Fluorescence Detector 分析仪器 (革命) Challenge 1 挑战 --- Identification confirmation Challenge 1False positive/negative ? However, only 2% is positive, confirmed by other method. --------------------------------------------------------------------- 17/18 False Positive! ***90%假阳性*** 36% positive 改进前 改进后 HPLC Separation 239.00 239.05 239.10 239.15 239.20 239.25 m/z 0 20 40 60 80 100 Relative Abundance 239.15181 C 11 H 19 O 2 N 4 6.50 ppm R = 15,000 Error = 6.50 ppm R = 80,000 0.32 ppm Resolution 分辨率 Pesticide Mixture in Horse Feed Matrix 239.00 239.05 239.10 239.15 239.20 239.25 m/z 0 20 40 60 80 100 Relative Abundance 239.15033 C 11 H 19 O 2 N 4 0.32 ppm 239.00 239.05 239.10 239.15 239.20 239.25 m/z 0 2