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Urine is the matrix of choice as it can be collected easily and in large volumes. The variations within the urine matrix can adversely impact chromatographic separation and LC-MS/MS signal. The present study demonstrates that a simple “dilute and shoot” method coupled with the high sensitivity QSight? 220 triple quadrupole mass spectrometer system eliminates many of the complexities of sample preparation without compromising quantitation quality.
The present research study provides a much simplified approach whereby a highly sensitive LC-MS/MS triple quadrupole mass spectrometer is used to measure directly the methadone and EDDP concentrations through the dried blood spot (DBS) samples.
The origin of statins dates back to the mid 1970’s when the Japanese biochemist, Akira Endo, isolated a factor from the fungus Penicillium citrinum which he identified as a competitive inhibitor of 3-hydroxy-3-methylglutarylcoenzyme A reductase (HMG-CoA reductase). This substance, which he named compactin or mevastatin, was the first statin to be administered to humans. Statins competitively inhibit HMG-CoA reductase, an enzyme involved in cholesterol synthesis, especially in the liver. Used to prevent cardiovascular disease and to lower cholesterol levels, atorvastatin is one of a number of synthetic statins routinely produced. It is now the most commonly prescribed statin medication. This application brief describes the robust HPLC analysis of the polar compound atorvastatin using a gradient which reaches 100% aqueous mobile phase conditions.
Opiates, originally derived from the opium poppy, have been used for thousands of years for both recreational and medicinal purposes.
This application note outlines a rapid LC-MS/MS research method utilizing the QSight? 220 triple quadrupole mass spectrometer. The developed method provides exceptional results for the quantitation of methotrexate in serum especially in terms of LLOQs and linearity.
Today, Warfarin is the most widely used anticoagulant in the world, used to thin the blood and prevent clots.1 It was discovered by chance when in the 1920’s cattle in the US were found to be bleeding to death having eaten mouldy hay from sweet clover crops.2 However, the exact identity of the substance causing the haemorrhaging was to remain unknown for many years. Over the coming years studies of the spoiled hay eventually led to the extraction of a compound which was later named dicoumarol. It was observed that this dicoumarol could not act as an anticoagulant on its own. It was only after it was metabolised byfungi that it exhibited anticoagulant properties. This explained why only spoiled hay caused the outbreak in the cattle. After further research, the synthesis of a more potent anticoagulant from dicoumarol, warfarin, was produced. Warfarin first commercial use was as a rat poison in 1948, followed by license for human use in 1953. This application brief illustrates the analysis of warfarin, Figure 1, using the Quasar AQ liquid chromatography phase.
Indoxyl sulfate is one of the most extensively studied solutes that accumulates in the plasma when the kidneys fail. Originally called "indican", it was first isolated by Obermayer and Popper in 1911. High concentrations of indoxyl sulfate in blood plasma are known to be associated with the development and progression of a number of pathological conditions including chronic kidney disease and vascular disease. The scientific literature documents the use of older generation C18 columns, using type A silicas. This application brief will illustrate the application of a new generation C18 column, based on type B silica, for the analysis of indoxyl sulfate, Figure 1, as part of a research study to measure the total levels in a simulated blood serum environment.
Prednisolone, Prednisone and Cortisone are commonly used steroids to treat a range of inflammatory conditions and autoimmune disorders. These synthetic derivatives of hydrocortisone were developed and approved for medicinal use as early as the 1940’s. American chemists first identified Cortisone as having a therapeutic benefit in the treatment of rheumatoid arthritis and it was commercialized by Merck in 1948. The first commercially feasible synthesis of prednisone was carried out in 1955 in the laboratories of the Schering Corporation. A C18 HPLC column can be used for the analysis of these synthetic steroids, but they are not well retained, and resolution is incomplete. This application brief will look at the differences in chromatography between the Quasar C18 and AQ phase chemistries for the analysis prednisolone, prednisone and cortisone.
Sulfa drugs are accredited as the first set of compounds to exhibit antibiotic properties used to prevent bacterial infections in humans. The first sulfonamide, trade named Prontosil, was developed by Bayer in 1932. The subsequent years saw rapid development of antibacterial drugs and by the 1940’s sulfanilamide was widely used. Though the medicine was relatively safe, allergic reactions such as skin rashes, fever and nausea were common place. With the introduction of less-toxic derivatives and especially with the mass production of penicillin, its use declined. These short acting synthetic sulfa drugs are effective against a wide range of pathogenic microorganisms and are now commonly used in veterinary medicine. Sulfathiazole administered to cattle in combination with penicillin and chlortectracyline has been shown to yield higher rates of weight gain and improved feed efficiency. This application brief illustrates the efficient separation of three sulfa drugs using the Quasar C18 HPLC column.
Measurement of metanephrines and normetanephrine in plasma is challenging due to the low physiological concentrations, their hydrophilic nature1, and time consuming traditional sample preparation. With use of the PerkinElmer QSight? 220 triple quadrupole mass spectrometer, LC-MS/MS analysis was performed using the recently advanced solid phase extraction (SPE) sorbent technology (“load, wash, elute”) method protocol. As a result low levels of ME and NOR are detectable in plasma with short sample preparation and LC run time. This LC-MS/MS method provides a fast, sensitive, accurate, and reproducible solution for the analysis of ME and NOR in plasma.
This application describes an analytical method for the chromatographic separation and quantitative monitoring of seven primary cannabinoids, including THC and THC-A, in cannabis extracts by HPLC with PDA detection. Naturally occurring cannabinoids, the main biologically active component of the cannabis plant, form a complex group of closely related compounds, of which 113 are known and 70 are well described. Of these, the primary focus has been on ?9-tetrahydrocannabinol (THC), as the primary active ingredient due to its pharmacological and toxicological characteristics, upon which strict legal limits have been enforced.