Then there were the chapters that I did bring in for Raman spectroscopy, acoustic emission, and effusivity.And now, we are looking at revising some of the waters chapters. 643 and 645 were originally devised as lab offline tests, but were revised to reflect the fact that you can do online monitoring. One of the things that I recognized early when I joined the USP, with respect to the PAT initiative, was the fact that the USP actually had the first online general chapter for process monitoring for pharmaceutical waters, published around 1997. Other chapters now under consideration by USPs general chapters committee focus on chemical imaging and chemometrics. EC - I think youre being a little modest about the work on1119. After all it was back in 1998-99 when you held the meeting and brought people from industry, academia and the USP together to propose a chapter.
If I remember correctly, you browbeat them into coming up with a useable document for submission in nine months. Compared to some of the committees that work on such things through several ice ages, I think that was rather commendable.GR - Other than the science that Ive always been involved in at the analytical level, I grasped very early the importance of understanding how people use a given technique and why they need to use that technique.
One of the things that 1119 had suffered from for many years was the fact that, while it was in the Compendium, it didnt receive much attention.Thats because it focused mainly on system suitability or system verification. It existed as a way for someone who wanted to implement NIR measurement, to know how to calibrate the wavelength for photometric accuracy and photometric precision. That would have been great if a lot of people were using NIR. But when the chapter existed [in that form], not that many people were using NIR. What they really needed to know, from an analytical point of view, especially if they were going to use the technique for pharmaceutical work, was How am I going to generate and validate a method? And the chapter really didnt answer that question. It instead answered the question I have an instrument. Does it measure something? EC - So the new chapter basically has some hints on how to do quantitative and qualitative validations? GR - "Identification, all the things that you, in your early days, actually taught the industry about what the techniques were useful for. And my work at Purdue, and yours, answered the questions: OK we know that NIR can be used to take this measurement. How do we validate it so that FDA and other regulators actually accept it? EC - The other thing was that you had been instrumental in getting the new NIR standards for USP because NIST had given up that standard. They no longer make it, yet it is required to have some traceable standard for any technique. The FDA really likes to have everything required for IQ, OQ, PQ, for method validation. For instance in chromatography, you need a USP standard to run against. Now for spectroscopy you have a USP standard to run against. GR - Absolutely. When I joined USP it became obvious that we needed to make the standards more useful, so that they went beyond merely answering questions that regulatory agencies could have regarding a submission. How could regulatory authorities independently verify that a person using the chapter and verifying suitability. How, for example, could FDA verify the fact that the suitability values reported back in some lab notebook stating that on a certain date, a given wavelength was tested. How could they verify that that the testing actually was done? EC- They couldnt. Its pretty much like standardized thermometers or anything else. Traceable is the key word. GR -Thats correct. And the void that was left by SRM 1920A, the previous NIST NIR standard that you referred to, needed to be filled by an improved 1119 Chapter. It really was a no brainer. EC - So youre doing this with multiple testing of standards on grating and Fourier Transform instruments? GR -The specification has not changed, its actually been expanded. When the original 1920A standard spec was originally tested, during a round robin of collaborative studies involving six equipment vendors, it specified three wavelengths, and established 1 nm and 1.5 nm wavelength specifications.
What weve done in the certification of the new standard that will be coming out shortly, is that were actually certifying standardizing seven wavelengths. The user, depending on which portion of the spectrum that he or she wishes to operate in, or even the whole spectrum, can choose any three wavelengths for qualifying any instrument for its intended use in measuring a process or product.EC Youve added talc to get a peak above 2000 nm? GR Some say that this may not extend the standards usefulness. Ive heard opinions, both pros and cons on the additional band above 2000, but its usefulness remains to be seen. I know that, for fiber optic work, you generally dont want to read anything above 2100 nm or so because of internal attenuation you get with the energy on the fiber optic material. If you go ahead and use this area of the spectrum for calibration sometimes youll get a lot of noise and scatter. But thats only a problem with fiber optic work. If someone is using a model for even, say, qualitative work, but using a direct hemispherical detection system, that end of the spectrum is useful up to 2500nm. I think they get an additional advantage with this extra peak.
Stay tuned tomorrow for reports on Day 1's general sessions and keynote speeches from FDA's Deputy Commissioner Dr. Janet Woodcock, Dr. Ajaz Hussain and Dr. Moheb Nasr.