scholarly journals Preparation of Antihypertensive Drugs in Biological Matrix with Solvent Front Position Extraction for LC–MS/MS Analysis

Molecules ◽  
2021 ◽  
Vol 27 (1) ◽  
pp. 205
Author(s):  
Kamila Jaglińska ◽  
Beata Polak ◽  
Anna Klimek-Turek ◽  
Robert Błaszczyk ◽  
Andrzej Wysokiński ◽  
...  
Keyword(s):  
Antihypertensive Drugs ◽  
Extraction Procedure ◽  
3D Printer ◽  
Tandem Mass ◽  
Biological Matrix ◽  
Solvent Front ◽  
Front Position ◽  
Quantitative Results ◽  
Matrix Components ◽  
Error Percentage

Solvent front position extraction procedure was used to prepare biological samples containing selected antihypertensive drugs (ramipril, lercanidipine, indapamide, valsartan, hydrochlorothiazide, perindopril, and nebivolol). Substances separated from the biological matrix components (bovine serum albumin) were quantified by means of liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Sample preparation process was performed with the use of a prototype horizontal chamber with a moving pipette driven by a 3D printer mechanism enabling a controlled eluent flow velocity. Application of this device was advantageous for simultaneous preparation of several samples for further quantitative analysis, with a synchronized reduction of manual operations and solvent consumption. Quantitative results obtained for the majority of the investigated antihypertensive drugs in a complex biological matrix were satisfactory. The values of the %RSD were around 5% for six of the seven substances (with the exception of indapamide). The method exhibits a suitable accuracy (the relative error percentage was below 10% for most drugs). The values of LOD and LOQ were in the range of 1.19 µg/L–8.53 µg/L and 3.61 µg/L–25.8 µg/L, respectively.

scholarly journals Solvent Front Position Extraction with Semi-Automatic Device as a Powerful Sample Preparation Procedure Prior to Quantitative Instrumental Analysis

Molecules ◽  
2019 ◽  
Vol 24 (7) ◽  
pp. 1358 ◽  
Author(s):  
Anna Klimek-Turek ◽  
Kamila Jaglińska ◽  
Magdalena Imbierowicz ◽  
Tadeusz Dzido
Keyword(s):  
Sample Preparation ◽  
Automatic Device ◽  
Preparation Procedure ◽  
3D Printer ◽  
Adsorbent Layer ◽  
Solvent Front ◽  
Front Position ◽  
Classical Procedure ◽  
Sample Preparation Procedure ◽  
Prototype Device

The new prototype device is applied to the Solvent Front Position Extraction (SFPE) sample preparation procedure. The mobile phase is deposited onto the chromatographic plate adsorbent layer by the pipette, which is moved, according to programmed movement path, by a 3D printer mechanism. The application of the prototype device to SFPE procedure leads to the increased repeatability of the results and significant reduction of the analysis time in comparison to the classical procedure of chromatogram development. Additionally, the new equipment allows use procedures that are not possible to run using the classic chromatogram development. In this paper, the results of manual and semi-automatic sample preparation with SFPE are compared and the possible application of this prototype device is discussed.

Rapid evaluation method for propofol abusing with hair by using centrifugal filter and liquid chromatography-tandem mass spectrometry

2020 ◽  
Vol 16 ◽  
Author(s):  
Jaesung Pyo
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Matrix Effect ◽  
Hair Sample ◽  
Extraction Procedure ◽  
The Body ◽  
Tandem Mass ◽  
Centrifugal Filter ◽  
Hair Samples

Background: Since propofol is rapidly metabolized and excreted from the body, it is not easy to quantify its intake in blood or urine sample over the time. In this case, the hair sample would be more advantageous to estimate during the abuse period. However, presence of protein and lipid in the hair sample could interfere extraction and be problematic during mass spectrometric analysis. Objective: The aim of this study is to develop the simple and less-time consuming method for extraction of propofol glucuronide by removing hair interferences with centrifugal filter. Method: Hair samples were washed and dissolved with sodiumhydroxide solution. This dissolved hair solution was applied to centrifugal filter and centrifuged. The filtrate was extracted with ethyl acetate and evaporated to dryness. The residue was reconstituted with methanol and analyzed by liquid chromatography coupled with tandem mass spectrometry. This developed analytical method was validated by testing of linearity, selectivity, accuracy, precision, recovery, matrix effect and stability of propofol glucuronide. Results and Discussion: The validation results showed good linearity over the concentration range of 0.5~500 pg/mg, with correlation coefficient of 0.9991. The LOD and LLOQ was 0.2 and 0.5 pg/mg, respectively. The intra-and inter-day precision and accuracy were acceptable within 14.5% for precision and 10.1% for accuracy. Similarly, the developed method revealed high sample recovery (>88%), low hair matrix effect (<10%) and highly-efficient extraction procedure. Conclusion: This well validated procedure was successfully applied to determine propofol glucuronide in rat hair sample and can be applicable, with high potential, in the field of forensic toxicology especially with increasing abuse and accidental overdose of propofol.

scholarly journals Quantitative Analysis of Pyrazines and Their Perceptual Interactions in Soy Sauce Aroma Type Baijiu

Foods ◽  
2021 ◽  
Vol 10 (2) ◽  
pp. 441
Author(s):  
Yan Yan ◽  
Shuang Chen ◽  
Yao Nie ◽  
Yan Xu
Keyword(s):  
Mass Spectrometry ◽  
Quantitative Analysis ◽  
Ultra Performance Liquid Chromatography ◽  
Alcohol Solution ◽  
Soy Sauce ◽  
Tandem Mass ◽  
Odor Thresholds ◽  
Quantitative Results ◽  
Odor Activity Value ◽  
The Impact

Pyrazines are important compounds in soy sauce aroma type Baijiu (SSAB). In this work, a total of 16 pyrazines were analyzed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS) in SSAB. The quantitative results showed that 2,3,5,6-tetramethylpyrazine, 2,6-dimethylpyrazine and 2,3,5-trimethylpyrazine were the three most concentrated pyrazines. The highest odor activity value (OAV) was determined for 2-ethyl-3,5-dimethylpyrazine. Quantitative analysis combined with descriptive sensory analysis revealed that sub-threshold pyrazines (2,3-dimethylpyrazine, 2,3-diethylpyrazine, 2,3-diethyl-5-methylpyrazine and 2-acetyl-3-methylpyrazine) are significantly correlated with the roasted aroma in SSAB. Our study focused on the impact of sub-threshold pyrazines on the perception of roasted aroma in SSAB. The effect of the sub-threshold pyrazines was detected by the addition of various pyrazines in SSAB samples, despite their sub-threshold concentrations. Furthermore, the presence of sub-threshold pyrazines in dilute alcohol solution resulted in a significant reduction in the odor thresholds of supra-threshold pyrazines. Sensory investigation indicated that pyrazines have a synergistic effect on the perception of roasted aroma. The results highlighted the contribution of some pyrazines to the roasted aroma in SSAB despite their sub-threshold concentrations.

Abstract P476: 8-Aminoguanosine Exerts Diuretic and Natriuretic Activity via Conversion to 8-Aminoguanine

Hypertension ◽  
2017 ◽  
Vol 70 (suppl_1) ◽  
Author(s):  
Edwin K Jackson ◽  
Zaichuan Mi
Keyword(s):  
Intravenous Administration ◽  
Sodium Excretion ◽  
Antihypertensive Drugs ◽  
Urine Volume ◽  
Systemic Circulation ◽  
Tandem Mass ◽  
Contralateral Kidney ◽  
New Class ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

We previously reported that 8-aminoguanosine and 8-aminoguanine are potent and efficacious K + -sparing diuretics/natriuretics that may represent a new class of antihypertensive drugs. Moreover, because these compounds are endogenous, they may have physiological roles. It is possible that the diuretic/natriuretic activity of 8-aminoguanosine is mediated mostly via conversion to 8-aminoguanine. To test this concept, we conducted 3 protocols in anesthetized rats. The 1 st protocol demonstrated that at 85 to 115 min post intravenous administration, both 8-aminoguanosine and 8-aminoguanine (33.5 μmol/kg) significantly increased urine volume [ml/min: 8-aminoguanosine from 0.3 ± 0.1 to 0.9 ± 0.1 (mean ± SEM; n=7); 8-aminoguanine from 0.3 ± 0.1 to 1.5 ± 0.2 (n=8)] and sodium excretion (μmol/min: 8-aminoguanosine from 12 ± 6 to 109 ± 21; 8-aminoguanine from 18 ± 8 to 216 ± 31). The 2 nd protocol showed that intrarenal artery infusions of 8-aminoguanosine (from 0.1 to 1 μmol/kg/min) did not affect urine volume or sodium excretion in either the ipsilateral or contralateral kidney. In contrast, intrarenal artery infusions of 8-aminoguanine significantly increased ipsilateral (but not contralateral) urine volume [at 1 μmol/kg/min from 0.2 ± 0.02 to 0.7 ± 0.1 (n=17)] and sodium excretion (from 24 ± 4 to 216 ± 31). In a 3 rd protocol we administered 8-aminoguanosine and 8-aminoguanine intravenously (33.5 μmol/kg) and measured renal interstitial (medulla) levels of 8-aminoguanosine and 8-aminoguanine using microdialysis combined with ultraperformance liquid chromatography-tandem mass spectrometry. Intravenous administration of 8-aminoguanosine and 8-aminoguanine similarly increased renal interstitial levels of 8-aminoguanine [ng/ml; 8-aminoguanosine from 4 ± 1 to 1025 ± 393 (n=6), and 8-aminoguanine from 2 ± 1 to 1069 ± 407 (n=6)]. Neither 8-aminoguanosine nor 8-aminoguanine affected renal interstitial levels of 8-aminoguanosine. Together these data clearly show that the renal effects of 8-aminoguanosine are not direct, but require conversion in the systemic circulation to 8-aminoguanine. If 8-aminoguanosine is physiologically important it should be viewed as a “pro-hormone.” As a pharmacological agent, it is best described as a “pro-drug.”

scholarly journals Pressurized Solvent Extraction with Ethyl Acetate and Liquid Chromatography—Tandem Mass Spectrometry for the Analysis of Selected Conazole Fungicides in Matcha

Toxics ◽  
2018 ◽  
Vol 6 (4) ◽  
pp. 64 ◽  
Author(s):  
Renata Raina-Fulton ◽  
Aisha Mohamad
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Solvent Extraction ◽  
Matrix Effects ◽  
Tandem Mass ◽  
Esi Ms ◽  
Signal Suppression ◽  
Target Analytes ◽  
Matrix Components ◽  
Pressurized Solvent Extraction

The extraction of powdered nutraceuticals is challenging due to the low water content and high concentration of matrix components that can lead to significant matrix effects in liquid chromatography-positive ion electrospray ionization-tandem mass spectrometry (LC-ESI+-MS/MS). In this study we assess the feasibility of using pressurized solvent extraction with ethyl acetate to reduce the co-extraction of polar matrix components. Pigment attributed to chlorophyll was removed with in-cell clean-up utilizing Anasorb 747, Florisil®, and C18. Visible inspection of the extracts showed that pigment was removed from matcha, a powdered green tea sample. Pressurized solvent extraction with in-cell clean-up can be utilized to remove pigments from powdered samples such as nutraceuticals. Average matrix effect of the 32 target analytes that observed mass spectrometric signal suppression or soft MS signal enhancement was −41 ± 19% with the majority of analytes having a protonated molecular ion with m/z of 250 to 412. As generally moderate signal suppression was observed for conazole fungicides and structurally related compounds analyzed by LC-ESI+-MS/MS, it is recommended that matrix matched or standard addition calibration is used for quantitation. Catachins, other polyphenols, and caffeine are expected to contribute to the matrix effects observed in LC-ESI+-MS/MS. Diniconazole, fenbuconazole, and tebufenozide were the only target analytes with severe MS signal enhancement. Low levels (0.002–0.004 mg/kg) of prothioconazole-desthio and flusilazole were detected, along with trace levels of tebuthiuron in matcha.

scholarly journals Determination of S-Adenosylmethionine and S-Adenosylhomocysteine in Plasma and Cerebrospinal Fluid by Stable-Isotope Dilution Tandem Mass Spectrometry

2000 ◽  
Vol 46 (10) ◽  
pp. 1650-1656 ◽  
Author(s):  
Eduard A Struys ◽  
Erwin E W Jansen ◽  
Kees de Meer ◽  
Cornelis Jakobs
Keyword(s):  
Mass Spectrometry ◽  
Cerebrospinal Fluid ◽  
Stable Isotope ◽  
Tandem Mass Spectrometry ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Internal Standard ◽  
Tandem Mass ◽  
Analytical Technique

Abstract Background: Available methods for the determination of nanomolar concentrations of S-adenosylmethionine (SAM) and S-adenosylhomocysteine (SAH) in plasma and cerebrospinal fluid (CSF) are time-consuming. We wished to develop a method for their rapid and simultaneous measurement. Methods: We used tandem mass spectrometry (MS/MS) for the simultaneous determination of SAM and SAH, with stable-isotope-labeled internal standards. The 13C5-SAH internal standard was enzymatically prepared using SAH-hydrolase and [13C5]adenosine. The method comprises a weak anion-exchange solid-phase extraction procedure serving as clean-up step for the deproteinized plasma and CSF samples. After clean-up, samples were injected on a C18 HPLC column, which was connected directly to the tandem mass spectrometer, operating in MS/MS mode. Results: In plasma samples, the intraassay CVs for SAM and SAH were 4.2% and 4.0%, respectively, and the interassay CVs were 7.6% and 5.9%, respectively. In CSF, the intraassay CVs for SAM and SAH were 6.8% and 6.9%, respectively, and the interassay CVs were 4.2% and 5.5%, respectively. Mean recovery of SAM and SAH for both matrices at two concentrations was 93%. Detection limits for SAM and SAH in samples were 7.5 and 2.5 nmol/L, respectively. Concentrations of SAM and SAH in plasma from healthy subjects were within the previously reported ranges. In 10 CSF samples, the mean concentrations (range) were 248 (137–385) nmol/L for SAM and 11.3 (8.9–14.1) nmol/L for SAH. Conclusions: SAM and SAH can be analyzed by MS/MS, taking optimal advantage of the speed and high sensitivity and specificity of this relatively new analytical technique.

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