Optimizing analytical precision in the identification of synthetic cathinones and isomers: a comparative assessment of diverse GC-MS operating parameters.

Analyzing new psychoactive substances (NPSs) in forensic laboratories present a formidable challenge globally. Within illicit drug analysis, gas chromatography-mass spectrometry (GC-MS) emerges as a robust analytical tool. This study endeavors to assess and compare peak resolution in the analysis of illicit drugs, specifically focusing on 21 synthetic cathinones, encompassing 9 cathinone isomers. Varied GC-MS operating conditions, including distinct GC-MS columns and thermal gradients, were systematically employed for the simultaneous analysis of these synthetic cathinones. The study utilized HP-1 nonpolar and HP-5MS low-bleed columns to achieve optimal analyte resolution through modulation of GC-MS oven conditions. Mass spectra were meticulously recorded within a mass-to-charge (m/z) range spanning from 40 to 500 in full scan mode. The data showed that the cathinone isomers slightly differed in retention times and mass spectra. The GC oven conditions affected the peak resolution for chromatographic separation even with the same column. The peak resolution improved using a slower thermal gradient heat speed with a prolonged analysis time. Conclusively, the interplay of GC columns and thermal gradients emerged as pivotal factors impacting peak resolution in the analysis of illicit drugs. These empirical insights contribute to a nuanced understanding of peak resolution dynamics and facilitate the identification of synthetic cathinones, including their isomers, in seized materials through the judicious application of GC-MS methodologies.

Simultaneous Determination and Stability Analysis of Ten New Psychoactive Substances including Synthetic Cathinones, Phenethylamines, and Ketamine Substitutes in Urine Using Liquid Chromatography-Tandem Mass Spectrometry.

Knowing the stability of drugs is important to ensure accurate and reliable results of drug concentrations. This study evaluated the stability of ten new psychoactive substances (NPSs) in urine and methanol/water at different storage temperatures. Quantitative analyses were performed using liquid chromatography-tandem mass spectrometry. Three replicates of each storage condition were analyzed at day 0 and after 7, 14-, 30-, 60-, and 90 days with storage at +25°C, +4°C, and -20°C. For each analyte, the percent difference at each time interval from day 0 was calculated for each storage condition. Para-methoxyamphetamine (PMA), para-methoxymethamphetamine (PMMA), deschloroketamine (DCK), and 2-fluorodeschloroketamine (2-FDCK) were stable in urine, even when stored for 90-day periods at various temperatures. For synthetic cathinones, the concentrations declined over time at room temperature (+25°C) in urine but were relatively stable in methanol solvent with 0.1% formic acid. The significant degradation was found at +25°C, and the most excellent stability was shown by samples stored at -20°C. Phenethylamines (PMA and PMMA) and ketamine substitutes (DCK and 2-FDCK) were relatively more stable than synthetic cathinones (mephedrone, butylone, pentylone, ephylone, 4-MEAPP, and eutylone).

Quantitation of serum 25(OH)D2 and 25(OH)D3 concentrations by liquid chromatography tandem mass spectrometry in patients with diabetes mellitus.

Vitamin D has been considered to regulate calcium and phosphorus homeostasis and to preserve skeletal integrity. Serum 25-hydroxyvitamin D (25(OH)D) is the best indicator of vitamin D levels. The association of serum 25(OH)D deficiency with increased risk of type 1 diabetes (T1DM) and type 2 diabetes (T2DM) is controversial. We investigated serum 25(OH)D2 and 25(OH)D3 levels in diabetes patients by using liquid chromatography tandem mass spectrometry (LC-MS/MS). Serum 25(OH)D2 and 25(OH)D3 levels were measured with liquid chromatography tandem mass spectrometry in electrospray ionization positive mode. Chromatograms were separated using an ACE5 C18 column on a gradient of methanol. The total 25(OH)D levels were calculated as the sum of 25(OH)D3 and 25(OH)D2 levels. A total of 56 patients with T1DM and 41 patients with T2DM were enrolled in this study. There were 42 and 28 non-diabetic, age-matched volunteers who participated as the T1DM controls and the T2DM controls, respectively. The total 25(OH)D levels were lowest in the 21-40 age group. The levels of both 25(OH)D3 and the total 25(OH)D were significantly higher in the T1DM and T2DM groups than in the controls (p < 0.01 in T1DM and p < 0.05 in T2DM group, respectively). The 25(OH)D2 levels were only significantly higher in T1DM patients than in the controls. The percentages of vitamin D deficiency (total 25(OH)D less than 20 ng/mL) in the T1DM, T2DM, the T1DM controls and the T2DM controls were 7.1%, 0%, 14.3% and 3.6%, respectively. The percentages of vitamin D insufficiency (total 25(OH)D less than 30 ng/mL) in the T1DM, T2DM, the T1DM controls and the T2DM controls were 26.8%, 7.3%, 54.8% and 17.9%, respectively. The percentages of vitamin D deficiency and insufficiency were significantly lower in the T1DM patients than in the T1DM controls (p < 0.01). In the present study, both type 1 and type 2 diabetes patients had higher serum 25(OH)D levels and lower percentages of vitamin D deficiency/insufficiency.

Role of Salivary Immune Parameters in Patients With Primary Sjögren's Syndrome.

BACKGROUND: Several factors, including clinical manifestations and laboratory data, have been used to evaluate the disease activity of Sjögren's syndrome (SS). We investigated saliva indicators of disease activity in primary SS patients. METHODS: We enrolled 138 Taiwanese patients with primary SS and 100 Taiwanese normal controls. Interleukin (IL)-6, IL-17A, tumor necrosis factor-alpha (TNF-α), and rheumatoid factor (RF)-IgA levels in saliva samples were measured using ELISA or fluorescent enzyme-linked immunoassay. Serum IgG, IgA, and IgM levels were measured by nephelometry. Erythrocyte sedimentation rate (ESR) was measured with an automatic ESR analyzer. The t-test and Pearson correlation test were used. RESULTS: IL-6 level was higher in primary SS patients than in normal controls (14.23±14.77 vs 9.87±7.32, P=0.012), but there were no significant differences in IL-17A, TNF-α, and RF-IgA levels. In primary SS patients, IL-6 level correlated weakly with ESR and IgG levels (r=0.252, P=0.015, and r=0.248, P=0.017, respectively), and TNF-α level correlated weakly with IgG level (r=0.231, P=0.024). CONCLUSIONS: IL-6 may play a role in SS pathogenesis. Saliva IL-6 might be an indicator of disease activity in primary SS patients.