Applications
- 410000012-A01Rapid Detection of the Low Dose API in Xanax Using Surface-Enhanced Raman Spectroscopy for Anti-Counterfeiting Purposes
The emergence of counterfeit prescription drugs has become a concern for the pharmaceutical industry. Because of the low concentrations of APIs found in pharmaceutical drugs, normal Raman spectroscopy is typically not sensitive enough to detect the API from the surface of a pill. In this study we develop a surface-enhanced Raman spectroscopy (SERS)-based approach to identify a low-dose of the API alprazolam in a Xanax tablet using a handheld Raman spectrometer. If no SERS peaks consistent with alprazolam are observed from a Xanax tablet, the pill is a suspected fake. The method demonstrates the power of SERS to quickly verify the presence of alprazolam in the tablet for anti-counterfeiting purposes.
- 410000030-APortable Transmission Raman Spectroscopy for At-Line Content Uniformity Testing of Pharmaceutical Tablets
Analytical methods to perform CU testing should ideally be fast, noninvasive and achieved with limited sample preparation. Recently, transmission near-infrared (NIR) spectroscopy and transmission Raman spectroscopy have both been explored as alternative methods for rapid and non-destructive on- and at-line CU testing with no sample preparation. Although quick and nondestructive, transmission NIR spectroscopy suffers from poor chemical selectivity and is sensitive to changes in the testing environment. Transmission Raman spectroscopy combined with chemometric modeling is quickly emerging as a valued technique for CU testing due to its high chemical specificity, which is particularly useful when dealing with complex pharmaceutical formulations that contain multiple components.
- 410000039-AQuantitative Analysis of Solutions Using a High Resolution Portable Raman Spectrometer
Ternary mixtures of aqueous sugar solutions are measured and multivariate models of the concentration of analytes developed using BWIQ software.
- 410000046-AQTRam® for Content Uniformity Analysis of Low-Dose Pharmaceutical Tablets
In this note, we use a model drug, acetaminophen, to demonstrate the capability of QTRam® to quantify low concentrations of API in compressed tablets.QTRam® is a compact transmission Raman analyzer designed specifically for content uniformity analysis of pharmaceuticals in solid dosage forms.
- 8.000.6010Inline sample preparation – An effective tool for ion analysis in pharmaceutical products
By means of azide analysis in Irbesartan a simple, fast, precise and accurate ion chromatographic method for the determination of traces of inorganic contaminants in pharmaceuticals is described. Traces of toxic azides in pharmaceutical products can accurately be determined in the sub-ppb range after Metrohm Inline Matrix Elimination using isocratic ion chromatography (IC) with suppressed conductivity detection. While the azide anions are retained on the preconcentration column, the interfering pharmaceutical matrix is washed away by a transfer solution, ideally consisting of 70% methanol and 30% ultrapure water. The analytical setup provides a well-resolved azide peak and thus alleviates the common drawback of excipient interferences, especially from the nitrate anion. Calibration with azide standards is linear over the range of 5…80 ppb, providing a coefficient of determination of 0.9995. The limit of detection (LOD) and the limit of quantification (LOQ) of azide in Irbesartan are 5 and 30 µg/L respectively; the relative standard deviations (RSD) for the peak area, peak height and retention time being smaller than 3.9%. Robustness testing involved variation of column oven temperature and composition of the transfer solution and, in terms of peak area, provided RSDs smaller than 2.8% and 3.1% respectively.
- 8.000.6024Fully automated sample preparation for the content determination of tablets
Benzbromaron is one of the main uricosuric drugs currently used. In addition to sophisticated and expensive LC-MS and GC-MS methods, benzbromaron can be effectively determined by titration with sodium hydroxide solution using a straightforward, fully automated sample preparation method. A high-frequency homogenizer comminutes one or three tablets within 90 or 120 s respectively. The overall analysis time is 8 minutes. Ten-fold determinations with one and three tablets resulted in a benzbromaron content of 99.2 and 98.7 mg per tablet respectively. Increasing the number of tablets from one to three lowers the RSD from 1.36 to 0.88%. These results show an excellent agreement with the benzbromaron content indicated by the manufacturer (approx. 100 mg/tablet).Besides the presented Titrando/homogenizer combination, the other two members of the 815 Robotic Soliprep Sample Processor family offer comprehensive sample preparation possibilities within the fields of IC, HPLC, ICP or voltammetry.
- 8.000.6026Determination of the water content in tablets by automated Karl Fischer titration
The water content of tablets determines the release of their active ingredients as well as their chemical, physical, microbial and shelf-life properties. Accordingly, the water content is of crucial importance and has to be accurately determined. This paper describes the straightforward determination of the water content using automated volumetric Karl Fischer titration (KFT). Tedious sample preparation steps are eliminated by using a high-frequency homogenizer that additionally serves as a stirrer. Prior to titration, the homogenizer comminutes the tablets directly in the KF solution. As the comminution process takes place directly in the hermetically sealed titration vessels, interference from atmospheric humidity does not occur. Even after 24 h in the vessels, the moisture content of four different tablet type samples was within 93…108% of the initially determined values. With a coefficient of determination of 0.99993 the KF method is highly linear for water amounts between 4 and 215 mg. For all investigated tablet types, KFT provides results that lie within the range expected by the manufacturer.
- 8.000.6051PC-controlled dosing and liquid handling
The 800 Dosino controlled by tiamo™ or Touch Control can be used universally for dosing and liquid handling tasks in both the analytical laboratory or directly in the synthesis laboratory. This poster looks at three typical liquid handling applications, the synthesis of metal-organic compounds, the preparation of standards, and the determination of pharmaceutical ingredients.
- 8.000.6078Water determination in pharmaceuticals using an automated Karl Fischer Oven Technique
The poster describes the water determination in pharmaceuticals using the Karl Fischer oven technique.
- 8.000.6089Automated sample measurement in Karl Fischer titration
This poster describes a method for automated and precise dosing of liquid samples into the Karl Fischer titration cell using Metrohm Dosino liquid handling technology. First, the titer was automatically determined with ultrapure water. The same dosing procedure proved valuable for the automated water determination in highly viscous water-glycol fluids and low-boiling organic solvents such as n-pentane. Lastly, the method copes with the labor-intensive and human error-prone suitability test stipulated in chapter 2.5.12 in the European Pharmacopoeia.