pharmaceutical impurity analysis solutions - Lcms-connect.com

3.2ANALYSIS OF INORGANIC IMPURITIESDetermination of elementalimpurities in pharmaceuticalingredients according toUSP procedures by AgilentICP-OES and ICP-MSbased solutionsThe new methodology for the preparation and analysis of pharmaceutical samplesdescribed in the draft General Chapters USP and provides anopportunity for pharmaceutical laboratories to update their methodology andinstrumentation to address the limitations of the current heavy metals limit test(USP). The robust plasma system on the Agilent 700 Series ICP-OES is capableof analyzing the most challenging samples, such as undiluted organic solvents andconcentrated salt solutions, to enable fast, accurate analysis which is free of complexsample digestion procedures (See Figure 16).64PPM2As 188.980Cr 267.716Ba 455.403Mn 257.610Co 238.892Se 196.026Sr 407.771Zn 213.85700 30 60 90 120 150 180 210Time (min)Figure 16. The robust plasma system of the Agilent 700 Series ICP-OES ensures the stable analysis of difficultsamples, such as the 5 % NaCl brine solution shown here. Agilent Technologies, unpublished results.In combination with closed-vessel microwave digestion and sample stabilizationusing HCl, the Agilent 7700x ICP-MS has been shown to be capable of determiningall regulated elements at low levels in typical pharmaceutical sample digests (SeeAgilent publication 5990-9365EN). Simple method development and routine operationare provided by the standard helium (He) mode method, which uses a single set ofconsistent instrument operating conditions for all analytes and samples. As requiredin USP, unequivocal identifi cation and verifi cation of analyte results is alsoprovided by the secondary (qualifi er) isotopes measured in He mode.Low limits of detection are particularly important for potentially toxic trace elementsdefi ned in USP, notably As, Cd, Hg, and Pb. Calibrations for these elements inHe mode are shown in Figure 17, together with Pd and Pt, which are representativemembers of the platinum group elements (PGEs) that must be monitored when addedas catalysts as per USP.24