From fundamentals in calibration to modern methodologies: A tutorial for small molecules quantification in liquid chromatography–mass spectrometry bioanalysis

Analytical techniques for screening of cannabis and derivatives from human hair specimens

“…140 Mass spectrometry can be easily coupled with other analytical techniques, such as liquid chromatography (LC-MS), gas chromatography (GC-MS), or capillary electrophoresis (CE-MS). 141 These hyphenated approaches offer enhanced separation capabilities and complementary information, enabling comprehensive sample analysis. Mass spectrometry instruments have high analysis speed, allowing for rapid data acquisition and high sample throughput.…”

Integrating a Multiple Isotopologue Reaction-Monitoring Technique and LC-MS/MS for Quantitation of Small Molecules: Ten Mycotoxins in Cereals as an Example

“…Over the past two decades, liquid chromatography coupled with triple quadrupole mass spectrometry (LC-MS/MS) and high-resolution mass spectrometry have attracted widespread popularity for mycotoxin determination due to their inherent specificity, sensitivity, and accuracy. ,, These techniques have emerged as the “gold standard” for multimycotoxin quantitative analysis. , Since mass spectrometry lacks inherent calibration, diverse calibration strategies have been developed to enhance accuracy and precision . Consequently, in the pursuit of a dependable analytical approach, the creation of calibration curves stands out as a pivotal phase. − The present state of research methods predominantly concentrated on individual mycotoxins or specific mycotoxin types, employing the conventional multisample external calibration curve (MSCC). , This approach involves introducing six nonzero concentrations into a blank matrix to perform the MSCC, enabling the back-calculation of the analyte’s concentration of interest . Nevertheless, when confronted with the simultaneous quantification of an array of compounds, the MSCC method proves laborious and time-intensive, primarily due to the extensive preparation of working standard solutions. , The one-point calibration (OPC) method simplifies the procedure by requiring just a single measurement point; its drawback is evident, that is, a lack of a second calibration point to characterize the instrument’s dynamic response adequately. , Typically, the OPC method is more suitable when the sample’s analyte concentration closely aligns with the value of the concentrations generated in the OPC.…”

“…Consequently, in the pursuit of a dependable analytical approach, the creation of calibration curves stands out as a pivotal phase. − The present state of research methods predominantly concentrated on individual mycotoxins or specific mycotoxin types, employing the conventional multisample external calibration curve (MSCC). , This approach involves introducing six nonzero concentrations into a blank matrix to perform the MSCC, enabling the back-calculation of the analyte’s concentration of interest . Nevertheless, when confronted with the simultaneous quantification of an array of compounds, the MSCC method proves laborious and time-intensive, primarily due to the extensive preparation of working standard solutions. , The one-point calibration (OPC) method simplifies the procedure by requiring just a single measurement point; its drawback is evident, that is, a lack of a second calibration point to characterize the instrument’s dynamic response adequately. , Typically, the OPC method is more suitable when the sample’s analyte concentration closely aligns with the value of the concentrations generated in the OPC. In essence, the existing calibration strategies boast both advantages and limitations. , This underscores the pressing need for the development of a novel calibration curve strategy aimed at optimizing the analytical performance of LC-MS/MS, thereby amplifying the precision, accuracy, and efficiency of quantitative analytical methodologies.…”

“…Nevertheless, when confronted with the simultaneous quantification of an array of compounds, the MSCC method proves laborious and time-intensive, primarily due to the extensive preparation of working standard solutions. , The one-point calibration (OPC) method simplifies the procedure by requiring just a single measurement point; its drawback is evident, that is, a lack of a second calibration point to characterize the instrument’s dynamic response adequately. , Typically, the OPC method is more suitable when the sample’s analyte concentration closely aligns with the value of the concentrations generated in the OPC. In essence, the existing calibration strategies boast both advantages and limitations. , This underscores the pressing need for the development of a novel calibration curve strategy aimed at optimizing the analytical performance of LC-MS/MS, thereby amplifying the precision, accuracy, and efficiency of quantitative analytical methodologies.…”

Matrix Effects in GC–MS Profiling of Common Metabolites after Trimethylsilyl Derivatization

“…A bias uniformly affecting the whole sample can be easily corrected by internal standards (or other simple normalization techniques such as maximum or median normalization). If the bias, however, affects individual sample composites differently, i.e., if not all target compounds in a biological extract correlate with a selected internal standard, a matrix effect of those cannot be reasonably explored, and the experiment might result in systematic errors [ 7 , 14 , 16 , 28 ]. In profiling analyses, many compounds, including unknowns, are typically quantified at once, and finding an appropriate number of suitable internal standards for the different compounds is a very ambitious (and possibly expensive) task [ 16 ], and specific strategies need to be developed.…”