5-Batch Analysis for Agrochemicals
In the agrochemical industry, five-batch testing (or preliminary analysis) is a pre-requisite for registration of an agrochemical to demonstrate its chemical equivalence. This analysis method requires five representative random production batches to be analyzed for the identification and quantification of all components present in the substance as manufactured. The five-batch analysis is performed to account for at least 98% of the composition of a technical grade active ingredient, and this characterization data is necessary to support TGAI registration. The study requires the analysis of five representative random production batches for the presence of significant impurities (≥ 0.1% w/w) and borderline impurities (0.1% > x ≥ 0.06%) to generate the product specification for global regulatory needs.
Application of 5-Batch Analysis
- Identify and quantify impurities within the production batches of substances
- Provide crucial information that is used to generate a agrochemical product specification
- A core requirement for any registration of the technical material
Figure 1. Structures of common agrochemicals and pharmaceuticals that interact with esterases. (Wheelock, C. E.; et al. 2008)
Five-Batch Analysis Process
BOC Sciences works with our clients to advise the best 5-batch testing approach for a new arochemical product or for an existing product that has undergone a change in the manufacturing process or manufacturing site.
Selection of five manufacturing batches
- Our experts follow many guidelines when performing analytical methods to provide information on toxicological relevant impurities.
- The five randomly selected batches must be at a point in the manufacturing process, after which no further chemical reactions are intended (aimed at producing or purifying the substance).
Analytical method development
- A comprehensive study of the manufacturing process help identify the nature of the impurities and select the appropriate analytical technique for analysis, therefore, before initiating the method development, our analytical chemists fully consider the the country of submission of dossier for the five-batch analysis.
- Once the analytical technique is identified, we then optimize a series of parameters such as the polarity or phase of the column, column temperature, etc.
- The combined set of optimized parameters will be defined as a suitable method for the next step of preliminary screening of five batches.
- Prior to method validation, the active ingredients of all known and unknown impurities are characterized by using 1H NMR, Mass and FTIR to demonstrate the respective structures.
Method validation
- For the method validation process, the parameters to be covered are linearity, LOQ, LOQ, precision and accuracy. After the validation of the method, the methodology is used to analyze the target five batches.
Results Analysis
- We provide the reports generated for 2D or 3D analysis including impurity identification and synthesis, active ingredient and impurity content determination.
2D and 3D Techniques of Chromatography
BOC Sciences supports a set of analytical methods or transfer and validate existing methodology using a wide range of equipment:
- Scanning of 5 batches using suitable techniques like GC-MS / LC-MS / LC-MS-MS / 3D HPLC / Ion Chromatography
- Identification and characterizations of actives and impurities by GC-MS / LC-MS / LC-MS-MS / 1H-NMR / 13C NMR
- Method validation in compliance with SANCO/OPPTS guideline parameters
- Quantitative analysis of all components by GC/HPLC/GC-MS/ LC-MS
Figure 2. Effect of time to test initiation and sample handling on acute permethrin toxicity. (Wheelock, C. E.; et al. 2008)
BOC Sciences Advantages
- Highly specialized technical and analytical services for the worldwide registration and regulatory compliance of agrochemicals
- Robust analytical testing programs that span from research and product development through the production process to final product
- Relies on broad industrial experience, ensuring that all of our work meets the high standards expected by our clients
- Our regulatory experts, toxicology consultants, scientists and inspectors will ensure that you receive maximum levels of guidance, testing and inspection you need.
Reference
- Wheelock, C. E.; et al. Applications of Carboxylesterase Activity in Environmental Monitoring and Toxicity Identification Evaluations (TIEs). Reviews of environmental contamination and toxicology. 2008. 195: 117-178.