Getting ready for
USP 232, 233 and 2232

Microwave-Assisted Sample Preparation and Determination of Elemental Impurities in Pharmaceutical Products


Are you ready for new United States Pharmacopeia 232, 233, and 2232 and also ICH Q3D pharma regulations considering inorganic elemental impurities?
We hope yes, but maybe you are not. Frequently pharma laboratories are a world of chromatographs used for organic analysis. Now we are moving for a room with inductively coupled plasmas with optical emission or mass spectrometers (you will get used to new acronyms: ICP OES and ICP-MS). Yes, you will have new analytical instruments in your lab. Together with ICPs, you will also be engaged in sample preparation. You will use new procedures for as complete as possible oxidation of organic compounds and destruction of excipients followed by the determination of elemental constituents liberated in the liquid phase. Microwave-assisted preparation in closed vessels will become an important ally. This is the topic of this book where two analysts talk about this new demand and how to get prepared for it. A Q&A style was adopted for making your reading easier and funnier. The authors hope you enjoy it.


  • Overview about USP <232>, <233>, and <2232>
  • Microwave-assisted sample preparation
  • Determination of elemental impurities using ICP-OES
  • Determination of elemental impurities using ICP-MS
  • Validation Procedure
How could I validate developed analytical procedures? How could I evaluate accuracy? How could I evaluate precision? How could I evaluate sensitivity? How could I evaluate specificity? How could I evaluate sample throughput?
Getting ready for USP 232, 233 and 2232


Joaquim A. Nóbrega
Joaquim A. Nóbrega received his Ph.D. from the State University of Campinas in 1992 and completed his postdoctoral training with Prof. Ramon Murray Barnes (University of Massachusetts, Amherst, MA, 1996) and with Prof. Bradley Todd Jones (Wake Forest University, Winston-Salem, NC, 2003). He is a Full Professor at the Department of Chemistry, Federal University of São Carlos (São Carlos, São Paulo State, Brazil) and is a Visiting Professor at the Faculty of Pharmacy, University of Concepción (Concepción, Chile). His main research interests are sample preparation in inorganic analysis, atomic absorption spectrometry, atomic emission spectrometry, and inductively coupled plasma mass spectrometry. He is a member of the Group for Applied Instrumental Analysis since its beginning in 1994. He has recently started the Institute GAIA of Spectrometry for increasing interaction with professionals working with sample preparation and inorganic analysis using spectrochemical methods with emphasis in inductively coupled plasmas.
Camillo Pirola
Camillo Pirola is Marketing and Business Development Manager at Milestone. After receiving his degree in Chemistry, Camillo joined Milestone in May 1991 as Application Chemist. His professional career does interlace with Milestone overall growth. Camillo became Application Manager, providing application support to all Milestone distributors around the world. In the late 90’s he became Area Manager for several Countries including Japan, Italy, the UK, Spain, Russia, India and Brazil. While retaining his position of Area Manager, Camillo took in the mid 2000’s the full responsibility for the Milestone marketing at global level. Since 2012 he is also Business Development Manager at Milestone. Camillo has contributed to several scientific papers and lectures and is often invited to give presentations, seminars and training courses worldwide.

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