Method and device for the quantitative analysis of solutions and dispersions by means of near infrared spectroscopy

Abstract

The present invention relates to a method for quantifying the composition of a product, with the following steps: irradiating the product with a radiation source in the near infrared range; receiving radiation which is reflected by or transmitted through the product, and providing an output signal corresponding to the intensity of the radiation received at a number of different wavelengths; determining whether or not the product lies within predetermined integrity criteria on the basis of the output signal using a mathematical method, wherein the product contains a solution or homogeneous dispersion, and the content of at least one substance contained in the dispersion or solution is quantitatively determined on the basis of the output signal., The present invention also relates to an apparatus for carrying out this method.

1 . A method for quantifying the composition of a product, comprising the steps of: 
 irradiating the product with a radiation source in the near infrared range;    receiving radiation which is reflected by or transmitted through the product, and providing an output signal corresponding to the intensity of the radiation received at a number of different wavelengths;    determining whether or not the product lies within predetermined integrity criteria on the basis of the output signal using a mathematical method,    wherein    the product contains a solution or homogeneous dispersion, and the content of at least one substance contained in the dispersion or solution is quantitatively determined on the basis of the output signal.    
   
   
       2 . The method of  claim 1 , wherein the product is moving.  
   
   
       3 . The method of  claim 1 , wherein the product contains a dispersion, and the at least one substance is present in the disperse and/or continuous phase of the dispersion.  
   
   
       4 . The method of  claim 1 , wherein the radiation transmitted through the product is received.  
   
   
       5 . The method of  claim 1 , wherein calibration is carried out at least once by quantitatively determining the content of the at least one substance in the solution or dispersion by means of an alternative method.  
   
   
       6 . The method of  claim 5 , wherein the alternative method is HPLC.  
   
   
       7 . The method of  claim 1 , wherein the determination step uses weighting factors.  
   
   
       8 . The method of  claim 7 , wherein the product contains a dispersion, and weighting factors which are found on the basis of a solution are used in the determination step.  
   
   
       9 . The method of  claim 8 , wherein the solution for finding the weighting factors and the dispersion contain the same substance to be quantitatively determined.  
   
   
       10 . The method of  claim 8 , wherein this substance contained in the dispersion is distributed between the continuous and disperse phases.  
   
   
       11 . The method of  claim 1 , wherein the product contains a dispersion which contains crystalline and/or dissolved insulin.  
   
   
       12 . The method of  claim 2 , wherein the moving product is a solution or dispersion in primary packaging.  
   
   
       13 . The method of  claim 12 , wherein the moving product is an insulin vial or insulin cartridge.  
   
   
       14 . An apparatus for determining the quantitative content of at least one substance in a moving product, which comprises a solution or homogeneous dispersion in a container, comprising 
 a radiation source, which emits radiation in the near infrared range, for irradiating the product;    a radiation reception device, which receives the radiation reflected by or transmitted through the product;    a spectrometer for receiving the radiation from the radiation reception device and for providing an output signal corresponding to the intensity of the radiation received at a number of different wavelengths;    a device for quantitatively determining the content of at least one substance contained in the dispersion or solution on the basis of the output signal.    
   
   
       15 . The apparatus of  claim 14 , wherein the spectrometer has a device for splitting the received radiation into a number of wavelengths for detection by a photodiode array.  
   
   
       16 . The apparatus of  claim 14 , wherein the source radiation source is a mercury halogen lamp.  
   
   
       17 . The apparatus of  claim 14 , wherein the radiation reception device also has an optical fiber which delivers the radiation emitted by the radiation source to the location of the product.  
   
   
       18 . The apparatus  claim 17 , wherein the radiation reception device has a converging lens.  
   
   
       19 . The apparatus of  claim 14 , wherein the determination device uses weighting factors.  
   
   
       20 . The apparatus of  claim 19 , wherein the weighting factors that are used are found on the basis of a solution.  
   
   
       21 . The apparatus  claim 14 , additionally comprising a calibration device, with which the quantitative content of the at least one substance can be determined by an alternative method.  
   
   
       22 . The apparatus of  claim 21 , wherein the calibration device comprises a high pressure liquid chromatograph.  
   
   
       23 . The apparatus of  claim 14 , additionally comprising a sorting device for rejecting the products which do not lie within the predetermined integrity criteria.  
   
   
       24 . The apparatus of  claim 14 , additionally comprising a device for homogenizing dispersions to be quantified.  
   
   
       25 . The apparatus of  claim 14 , additionally comprising a device for detecting the product position.  
   
   
       26 . A method for line control of product units in the production, filling and/or packaging of solutions or dispersions for pharmaceutical purposes comprising use of the apparatus of  claim 14 .  
   
   
       27 . A method of filling solutions and dispersions, comprising use of the apparatus of  claim 14.