Quantification of 25 hydroxy vitamin D2 and 25 hydroxy vitamin D3 in human serum samples using triple quadrupole tandem mass spectrometry

2008 ◽  
Vol 41 (14-15) ◽  
pp. 1287
Author(s):  
S.C. Leonard ◽  
L.M. Sapp ◽  
J.D. Miller ◽  
J Krol ◽  
J. Brown
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Human Serum ◽  
Vitamin D3 ◽  
Tandem Mass ◽  
Vitamin D2 ◽  
Triple Quadrupole ◽  
Serum Samples ◽  
Human Serum Samples

A Selective and Sensitive Gas Chromatography-Tandem Mass Spectrometry Method for Quantitation of Synthetic Musks in Human Serum

2020 ◽  
Vol 103 (6) ◽  
pp. 1461-1468
Author(s):  
Guru Prasad Katuri ◽  
Xinghua Fan ◽  
Shabana Siddique ◽  
Cariton Kubwabo ◽  
Ivana Kosarac ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Serum ◽  
Solid Phase ◽  
Consumer Products ◽  
Tandem Mass ◽  
Serum Samples ◽  
Synthetic Musks ◽  
Synthetic Musk

Abstract Background Synthetic musk compounds are widely used as fragrances in many consumer products; however, information on human exposure and health effects is limited. Also, analytical methods for their quantification in biological matrices are limited. Objective In this study, an integrated method was developed and validated for the analysis of selected synthetic musk compounds in human serum. Method The method is based on liquid-liquid extraction (LLE), sample clean-up by solid-phase extraction (SPE), and separation and detection by gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). Results The method demonstrated good recoveries (86–105%) and high sensitivity, with low method detection limits (MDLs) ranging from 0.04 to 0.17 µg/L. The method was applied to the analysis of 10 synthetic musk compounds in 40 serum samples collected from Canadian women aged 20–44 years (20 individual samples collected in 2014 and 20 pooled samples collected in 2006). The most commonly detected compound was Galaxolide (HHCB), with median concentrations of 0.59 µg/L in samples collected in 2006, and 0.34 µg/L for samples collected in 2014. Musk ketone (MK) was not detected in any of the samples collected in 2006, but was detected in 60% of the samples collected in 2014 with a median concentration of 0.29 µg/L. Tonalide (AHTN) was detected in only one sample above its MDL (0.12 µg/L). Conclusions This is the first study in Canada to report levels of synthetic musks in human. The data generated from this study has been used in risk screening assessment by Environment and Climate Change Canada and Health Canada.

scholarly journals Determination of glyphosate and glufosinate in human serum by monospin TiO extraction and liquid chromatography–tandem mass spectrometry

2020 ◽  
Vol 32 (1) ◽  
pp. 10-15
Author(s):  
Takeshi Saito ◽  
Akira Namera ◽  
Tomoatsu Tsuji ◽  
Wataru Noguchi ◽  
Sadaki Inokuchi
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Serum ◽  
Accurate Determination ◽  
Tandem Mass ◽  
Serum Samples ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

We developed and validated an assay for determination of glyphosate (GLYP) and glufosinate (GLUF) in human serum. Serum samples were extracted by using a MonoSpin® TiO column and analyzed by liquid chromatography–tandem mass spectrometry (LC–MS/MS). MonoSpin® TiO tends to specifically bind to phosphate groups. The assay was linear over a concentration range of 1–250 μg/mL. The recoveries for the 2 compounds were 1.6%–2.3%. The intra- and inter-day variations were <15%. Precision and accuracy were 5.6%–12.7% and 97.0%–103.9%, respectively. The validated method was applied to quantify the GLYP and GLUF content in the serum of GLYP and GLUF-poisoned patients. In conclusion, the method was successfully applied for accurate determination of GLYP and GLUF in serum obtained from patients with GLYP and GLUF poisoning.

Determination of Vitamins D2 and D3 in Infant Formula and Adult Nutritionals by Ultra-Pressure Liquid Chromatography with Tandem Mass Spectrometry Detection (UPLC-MS/MS): First Action 2011.12

2012 ◽  
Vol 95 (3) ◽  
pp. 577-582 ◽  
Author(s):  
Jack Stevens ◽  
Dawn Dowell
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Infant Formula ◽  
Vitamin D3 ◽  
Tandem Mass ◽  
Vitamin D2 ◽  
Mass Spectrometry Detection ◽  
Method Performance

Abstract The method for the “Determination of Vitamins D2 and D3 in Infant Formula and Adult Nutritionals by Ultra-Pressure Liquid Chromatography with Tandem Mass Spectrometry Detection (UPLC-MS/MS)” was adopted as AOAC Official First Action during the “Standards Development and International Harmonization: AOAC INTERNATIONAL Mid-Year Meeting” held June 29, 2011. During the meeting, an Expert Review Panel (ERP) evaluated the available validation information against standard method performance requirements (SMPRs) articulated by stakeholders. The method, approved by the ERP, is applicable for the determination of vitamin D (total vitamins D2 and D3). A range of products had been tested during a single-laboratory validation study. The products included butter, National Institute of Standards and Technology SRM 1849, eggs, cheese, yogurt, ready-to-eat cereal, bread, mushrooms, and tuna. The testing of the method established linearity in the range of 0.005–50 μg/mL. The recovery range was 93.4–100.9% for vitamin D2 and 102.4–106.2% for vitamin D3. The LOD and LOQ for vitamin D2 were reported as 0.20 and 0.61 μg/100 g, respectively; for vitamin D3, the reported values were 0.47 and 1.44 μg/100 g, respectively. The method met the SMPRs set by the Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN). It was, therefore, decided that the method was appropriate for Official First Action Method status.

scholarly journals Development and validation of a productive liquid chromatography-tandem mass spectrometry method for the analysis of androgens, estrogens, glucocorticoids and progestagens in human serum

2021 ◽  
Author(s):  
Michele Iannone ◽  
Anna Pia Dima ◽  
Francesca Sciarra ◽  
Francesco Botrè ◽  
Andrea M. Isidori
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Human Serum ◽  
Reversed Phase ◽  
Tandem Mass ◽  
Triple Quadrupole Mass Spectrometer ◽  
Serum Samples ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Adrenal and gonadal disorders are very often coupled, due to common etiology or pathophysiology. We present the development, validation and application of a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the simultaneous analysis of androgens (androstenedione (A4), testosterone (T), dihydrotestosterone (DHT), and dehydroepiandrosterone sulfate (DHEA-S)), estrogens (estrone (E1), estradiol (E2), estriol (E3)), glucocorticoids (cortisol (F), cortisone (E), corticosterone (B), 11-deoxycortisol (S), 21-deoxycortisol (21DF), 11-deoxycorticosterone (11DB)), and progestagens (progesterone (P4), 17α-hydroxyprogesterone (17OHP4) and 17α-hydroxypregnenolone (17OHP5)) in human serum for clinical use. Samples (250 μL of matrix) spiked with isotopic labelled internal standards were extracted with tert-butylmethyl ether (TBME) prior to LC-MS/MS analysis. The chromatographic separation of the underivatized endogenous steroids was achieved on a reversed-phase column (C18 Zorbax Eclipse Plus) using a methanol-water gradient. The LC column was coupled to a triple quadrupole mass spectrometer equipped with an electrospray (ESI) source operating both in positive and in negative mode, with acquisition in multiple reaction mode. The method was validated using surrogated matrices and human serum samples. The proposed method was proven to be specific for all the considered steroids; and linearity was also assessed (R2 > 0.99) in the ranges of quantification investigated. The lower limits of quantification (LLOQs) were in the range of 10 - 400 pg/mL depending on the target steroid. Accuracy was in the range 80 - 120% for all the target compounds, the extraction recovery was higher than 65% for all the steroids considered and no remarkable matrix effect, expressed in terms of ion enhancement and ion suppression, was observed. To test the reliability of the developed and validated method, the analysis of serum samples collected from ten healthy subjects (5M/5F) was performed. In the clinical settings there is a growing need to develop accessible methods for full steroid hormone profiling. The dynamic link between steroidogenic glands and liver enzymatic processing (activation and clearance) attributes to the profile a much greater clinical meaning than a set of individually measured hormones. The presented method can be used to identify trajectories of deviation from the concentration normality ranges applied to disorders of the gonadal and adrenal axes.

Ultra-High-Performance Liquid Chromatography-Isotope Dilution Tandem Mass Spectrometry for the Determination of Phthalate Secondary Metabolites in Human Serum Based on Solid-Phase Extraction

2019 ◽  
Vol 102 (1) ◽  
pp. 271-277 ◽  
Author(s):  
Hongjian Miao ◽  
Yue Huang ◽  
Chao Ma ◽  
Jingguang Li ◽  
Yunfeng Zhao ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Solid Phase Extraction ◽  
Human Serum ◽  
Solid Phase ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Human Serum Sample ◽  
Serum Samples

Abstract Background: A multitude of biomonitoring analytical methods are applied in urinary detection, but few are applicable to phthalate metabolites in human serum, and those that are invariably involve complex operation. Objective: To develop a novel method for the determination of phthalate monoesters in human serum using solid-phase extraction (SPE) and ultra-HPLC (UHPLC)-tandem mass spectrometry for multiple human serum sample determination. Method: Analytes in serum samples were extracted and purified with a novel SPE cartridge named Prime HLB and then directly injected and analyzed without eluent redissolution. After sample extraction and cleanup, 11 phthalate monoesters were separated on a C18 chromatographic column in UHPLC. Among them, mono-isobutyl phthalate and mono-n-butyl phthalate, a pair of isomers, were successfully separated. Results: Lower LODs of the 11 monoesters in 0.5 mL human serum were in the range of 0.03–3 ng/mL, and lower LOQs accordingly ranged from 0.1 to 10.0 ng/mL. Recoveries from spiked bovine serum samples were in the range of 95.3–109.9%, and RSDs were 8.0–12.0%. Intra- and inter-day recoveries were in the range of 94.1–115.7%, with RSDs &lt;13.7%. Conclusions: The proposed method has been proved to be rapid, simple, accurate, and sensitive, so that it may potentially be used for high-throughput biological monitoring with high efficiency and precision. Highlights: Sample pretreatment does not require eluent drying and redissolution. Mass losses of analytes are avoided. Operational procedures are easy and rapid. The method has proved applicable for 11 phthalate metabolites in multiple human serum sample determinations.

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