Pharmaceutical analysis required sample volumes

With the availability of less expensive and more dependable commercial instruments, liquid chromatography coupled to mass spectrometry is quickly becoming the industry standard. However, the role of electrochemistry in pharmaceutical analysis has been well defined, and will likely continue to be preferentially employed in applications where low analyte concentrations, small sample volumes, or complex sample matrices requiring high specificity challenge the analytical method. 

Stage that requires high efficiency as well as speed, due to the complexity of the sample matrix, and hence it is particularly challenging to achieve the goals. Therefore, the development of a rapid, sensitive, and reproducible method has been required for separation and determination of capsaicinoid compounds. The addition of ultraperformance liquid chromatography-mass spectrometry (UPLC-MS) method fulfilled these aforementioned demands and showed some complementary advantages to the conventional HPLC-MS, u-HPLC methods in terms of shorter analysis times, low sample volume, and much improved sensitivity [71]. Therefore, nowadays this UPLC-MS technique is routinely performed in pharmaceutical industries and related contract research institutes, laboratories concerned with biochemistry, biotechnology, environmental analysis, natural product research, and several other research fields. The UPLC-MS method has successfully been applied for the determination of n-DHC, C, DHC, h-C, and h-DHC present in the varieties of hot peppers [71]. 

IEC continues to have numerous applications to the detection and quantification of various inorganic ions.1 1 This is particularly true in water analysis.5-14 Inorganic ions in a variety of other sample types, such as food and beverages,1518 rocks,19-23 biological fluids, (blood, urine, etc.),24-31 pharmaceutical substances,32 33 concentrated acids,34 alcohols,35 and cleanroom air36 have also been analyzed by IEC. IEC has also been employed in isotopic separation of ions,37 including the production of radioisotopes for therapeutic purposes.3839 Typical IEC sample matrices are complex, and may contain substances that interfere with measurement of the ion(s) of interest. The low detection limits required for many IEC separations demand simple extraction procedures and small volumes to avoid over-dilution. Careful choice and manipulation of the eluent(s) may be needed to achieve the desired specificity, especially when multiple ions are to be determined in a single sample. 

HPLC has more or less supplanted GC as a method for quantifying drugs in pharmaceutical preparations. Many of the literature references to quantitative GC assays are thus old and the precision which is reported in these papers is difficult to evaluate based on the measurement of peak heights or manual integration. It is more difficult to achieve good precision in GC analysis than in HPLC analysis and the main sources of imprecision are the mode of sample introduction, which is best controlled by an autosampler, and the small volume of sample injected. However, it is possible to achieve levels of precision similar to those achieved using HPLC methods. For certain compounds that lack chromophores, which are required for detection in commonly used HPLC methods, quantitative GC may be the method of choice, for analysis of many amino acids, fatty acids, and sugars. There are a number... 

In comparison with HPLC, CE techniques are better adapted to highly polar compounds, which are often difficult to analyze in chromatography. Additionally, analysis time in CE techniques is shorter than in HPLC and efficiency is higher than in the latter. Also, it is worth noting the low amounts of solvents (mainly alcohols) and buffers required and the minor volumes of sample needed. Despite all these evident advantages, CE techniques have not replaced HPLC in industrial applications. Although at present there is no doubt about the robustness of CE, the reticence of pharmaceutical companies to broadly use this technique may be related to its relatively poor limit of detection. 

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