Overview
In the agrochemical industry, pesticide discovery and development require stringent adherence to regulatory standards. One of the imperative steps in achieving this is the 5-batch analysis, a crucial quality control process that includes testing samples from five separate batches (or intervals in a continuous process) of a pesticide product. It ensures the chemical equivalence, consistency, and potency of the technical product and, assesses its composition (active ingredient, relevant impurities, significant impurities, and other possible constituents like residual solvents, metal contaminants, etc.) and adherence to reference specifications of regulatory standards. This analysis is a critical step in the registration of a new or a generic version of an existing agrochemical product and hence plays a pivotal role in safeguarding both agrarian yields and environmental integrity. At its core, it serves as a reliability test, determining product quality required for global regulatory compliance.
Selection Criteria for Batches
The most important criteria for the selection of the five batches are that they should reflect commercial conditions and are produced at pilot plant or commercial scale (minimum 5 kg). Generally, laboratory production runs are not acceptable, however, if supported by relevant commercial batches they may be considered. Additionally, it is advisable to avoid batches produced at a different physical site from the proposed approval location and, analyzing batches older than 5 years is not endorsed.
The Process
The 5-batch analysis is typically performed to Good Laboratory Practice (GLP) standards. Globally, the Food and Agriculture Organization of the United Nations (FAO) and the World Health Organization (WHO) provide guidelines and specifications for assessing the quality and consistency of agrochemicals. However, the specifics of the analysis vary according to the specific regulations and guidelines of the country where the product is being registered (see image below)
The 5-batch analysis aims to provide a robust framework for demonstrating adherence to regulatory standards set forth by governing bodies and encompasses the following steps:
1Preliminary screening:
The first and the most important step of the five-batch analysis is called screening analysis, followed by quantification and identification of the active ingredient and then the impurities (significant and relevant). Analytical techniques like 2D-HPLC, 3D-HPLC, GC-MS, LC-MS, ion chromatography and ICP-OES are used to screen the pesticide batches.
2Impurity identification, structure elucidation and isolation:
Any impurity - significant impurities ≥0.1% w/w, borderline impurities ≥ 0.06% w/w and toxicological relevant impurities are identified via spectroscopy and/or chromatography techniques like nuclear magnetic resonance (NMR), infrared spectroscopy (FT-IR) LC-MS-MS, mass spectrometry, etc. Contaminants found during the screening procedure are separated by additional analysis.
3Analytical method development and validation:
To quantify the active ingredients and impurities present in a pesticide batch, the development of analytical methods is essential. The routine procedure comprises the selection of appropriate analytical techniques, optimization of instrument parameters, and establishing approaches for suitable sample preparation. Next, the methods developed are validated according to the regulatory test guidelines.
4Quantitative analysis:
The active ingredient and all other constituents (such as solvents and contaminants) are quantitatively analyzed using ion chromatography, GC (FID), and HPLC along with the reference standards.
NOTE: Availability of reference standards is necessary for characterization of the active ingredients and impurities. In addition, qualitative and quantitative checks are performed through all stages of the process, ensuring accuracy, reliability, and compliance.
Why Intox?
At Intox, an Aragen Company, we specialize in five-batch analysis for the agrochemical industry. Here’s what sets us apart:
- Expertise: Our team of chemists and toxicologists ensures consistency and compliance with global regulatory directives.
- Experience: Over 40 five-batch studies have been successfully conducted on 25 different compounds of diverse properties, including challenging compounds like aluminum phosphide and zinc phosphide.
- Facility: Our State-of-the-art instrumentation provides access to a broad range of analytical instruments ensuring accurate testing and analysis.
- Customization: We tailor each step of the process to meet regulatory and specific requirements.
- Advancement: Partner with us to stay ahead in the evolving agrochemical landscape.
