|
簡體中文|
English| Launch：2022-07-04 |
Process Analytical Technology (PAT) originated in the July 2001 ACPS discussion. In 2004, the US FDA published an industry guideline on PAT - "PAT - A Framework for the Development, Production and Quality Assurance of Innovative Drugs", which clarified the status and role of PAT.
FDA believes that PAT is a system that integrates design, analysis and production control through real-time (that is, in the process) detection of key parameters and performance indicators related to raw materials, materials in production, and processes, and is similar to traditional quality assurance methods. ratio, has a very clear advantage in ensuring the quality of the final product.
Identification of chemical reaction components (reactants, intermediates, products, by-products, etc.)
Degree of chemical reaction (onset, rate/dynamics, concentration change, end point, etc.)
Chemical reaction kinetics and mechanism studies
Control of key process parameters (critical conditions, safety conditions)
Process efficiency and error-free rate (quality, repeatability, yield, etc.)
O2, H2O sensitive, unstable reaction mixture
Highly toxic, hazardous, explosive reaction mixture
low/high temperature, pressure
No disturbance, immersion, material loss
Take timely action
Reduce cycle time
Improve efficiency and reduce costs
Reduce impurity yield and improve product quality
Online Raman spectroscopy is widely used in process analysis, and has many applications in pharmaceutical reaction endpoint monitoring, impurity control, process research, purification process control, and preparation production process quality control.
The application of aspirin is limited clinically by the impurity component - salicylic acid, which is a residual reactant due to incomplete acetylation in the production process, which is toxic to the human body and is prone to salicylic acid reaction. exhaustion or even death. Therefore, it is very necessary to monitor the progress of the reaction in the synthesis of aspirin.
Testing process
1) Use PR785-7031-100X110-1200-25 to build an online Raman detection system for monitoring the synthesis process of aspirin;
Laser power: 400mW;
Wavelength: 785nm;
Integration time: 2000ms.
2) Collect the Raman spectrum from 0-30 min of reaction, and combine the spectral preprocessing and the vector angle algorithm to obtain the change trend graph of the angle with time;
2) Taking aspirin as an example, with the progress of the reaction, the included angle value gradually decreases, and the included angle value decreases to the minimum at 15 minutes, and after 15 minutes, the included angle value does not change, indicating that the reaction process has ended.
The online Raman technology can realize the process tracking of the reaction of the aspirin synthesis process, confirm that the reaction time is about 15 minutes, reduce the probability of residual reactant (salicylic acid), and ensure the quality of the finished drug product.
Application of Online Raman Technology in Chemical Industry
PX is an important basic chemical raw material, which mainly provides raw materials for terephthalic acid (PTA); PTA is a raw material for producing polyester and has a wide range of uses.
Adsorption and separation of PX from mixed xylene is the main method for producing PX at present. In order to ensure the purity and yield of PX, the PX production process needs to know the composition of the stream in real time and accurately, so as to provide guidance for the process operation.
The traditional gas chromatography has a slow detection speed and cannot simultaneously detect the changes in the flow components of the adsorption tower circulating line. The online Raman spectroscopy technology has the advantages of accuracy, rapidity, simple operation, on-site maintenance-free, clean and environmental protection, etc. It is especially suitable for aromatic isomerism. Rapid analysis of the body.
1. Collect Raman spectra of pure substances, and the modeling spectrum can be selected from 680~880cm-1.
2. Collect the spectrum of the mixed components, determine the content of the mixed components by GC, and use statistical regression to establish a quantitative model.
3. Model verification: A group of circulating fluid samples (24 samples) were collected, and the Raman analysis values were compared with the GC analysis values.
4. Practical application: PX with higher purity can be obtained above 15 plates.
Methanol gasoline refers to a new type of environmentally friendly fuel that is prepared by national standard gasoline, methanol and additives according to a certain volume (mass) ratio through a strict process. It is a fuel substitute for automobiles and an important part of new energy.
The most common is methanol gasoline with a methanol content of 15%, referred to as M15 methanol gasoline. The use of M15 methanol gasoline does not require modification of automobile engines, and it has been popularized and used in some parts of the country, and the market prospect is very optimistic.
Therefore, for methanol gasoline production enterprises, in the process of preparing methanol gasoline, there is an urgent need for a fast, accurate and suitable online operation detection instrument to guide stable production and achieve the purpose of optimizing benefits.
Since the operating room is far away from the site, a set of quartz optical fibers with a length of 200 m and a diameter of 100 μm are used to connect the 785 probe on the industrial site with the spectrometer host in the operating room.
在線檢測系統(tǒng)分析誤差在± 1% 范圍內(nèi)
甲醇含量的重復(fù)性偏差不超過 0.5%
Raman online monitors the bioreactor media components such as glucose, lactate, amino acids, etc.
For example, the online Raman monitoring system composed of Portman series refrigeration Raman spectrometers and RPB immersion probes has high sensitivity and low noise level, and is especially suitable for Raman signal detection of online reaction systems;The immersion probe has the characteristics of high temperature resistance, pressure resistance, corrosion resistance, etc., and is competent for working under extreme reaction conditions.
Features:
Refrigerated detectors are used, with low noise level, especially suitable for long integration time detection of weak light signals; area array detectors have high sensitivity and improve signal-to-noise ratio;
High resolution: minimum up to 2.5 cm-1;
Rich software functions: configure rich spectral processing and analysis algorithms, and choose cloud spectral data management;
Complete sampling accessories: It can meet various complex scenarios such as micro-area imaging and online reaction monitoring;
Portable, fast, and simple to build: You can quickly build a product portfolio suitable for the application according to the scene.
Features:
Can withstand corrosive liquids, acid and alkali resistance;
The front-end Hastelloy probe and focusing lens can be replaced;
The pigtail can withstand more than 50N pulling force and is not easy to be damaged；
The main body can withstand high temperature up to 80℃, and the front end can withstand high temperature of 200℃;
Flanges of different specifications can be welded according to customer requirements, supporting DN15, DN25 and DN32;
Explosion-proof joints can be configured according to customer requirements.
