The continuous exchange of chemicals with blood and the non-invasive collection make saliva an interesting specimen for clinical applications, from the detection of biomarkers to the new –omic sciences in medicine. However, saliva sampling is challenging because the suitability of the collection method for the analyte of interest is either poorly investigated or, more often, not mentioned at all in most publications. This review reports a critical evaluation of the most common procedures for saliva sampling and a description of the off-the-shelf sampling devices. Their suitability for bioanalytical applications and salivary biomarkers detection, e.g. representativeness of the sample, sampling feasibility, analyte recovery, and sample amount, is discussed.

Saliva sampling: Methods and devices. An overview

Liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) is one of the most prominent analytical techniques owing to its inherent selectivity and sensitivity. In LC/ESI-MS/MS, chemical derivatization is often used to enhance the detection sensitivity. Derivatization improves the chromatographic separation, and enhances the mass spectrometric ionization efficiency and MS/MS detectability. In this review, an overview of the derivatization reagents which have been applied to LC/ESI-MS/MS is presented, focusing on the applications to low molecular weight compounds.

Derivatization reagents in liquid chromatography/electrospray ionization tandem mass spectrometry.

Chemical derivatization for enhancing sensitivity during LC/ESI–MS/MS quantification of steroids in biological samples: a review

The life of a human female is characterized from teenage years by monthly menstruation which ceases (the menopause) typically between the age of 40 and 60 years. The potential for reproduction declines and ceases as the ovaries become depleted of follicles. A transition period in mid-life, for 2 to 10 years, when menstruation is less regular is called the perimenopause. The menopause is associated with a significant decline in plasma concentrations of sex hormones, an increase in the concentrations of the gonadotrophins and changes in other hormones such as the inhibins. These changes are superimposed with effects of aging, social and metabolic factors, daily activity and well-being. Although the menopause is entirely natural, in some cases ovarian failure can occur earlier than usual; this is pathological and warrants careful biochemical investigations to distinguish it from conditions causing infertility. Elderly females are affected by a range of clinical disorders including endocrine, cardiovascular, skeletal, urogenital tract and immunological systems, body mass, vasomotor tone, mood and sleep pattern. Reference intervals for many diagnostic biochemical tests for the menopause need to be used when interpreting results in clinical investigations for patient management. The standardization and harmonization of assays are being addressed. Many women now choose to develop their career before bearing children, and the health service has had to change services around this. This review does not cover screening for and tests during pregnancy. The review is timely since the population is aging and there will be more demand on healthcare services.

https://journals.sagepub.com/doi/pdf/10.1177/0004563217739930

Biochemistry of the menopause.

LC with atmospheric pressure ionization MS is essential to a large number of quantitative bioanalyses for a variety of compounds, especially nonvolatile or highly polar compounds. However, in many instances, weak ionization, poor LC retention and instability of certain analytes hinder the development of the LC-MS/MS method. Chemical derivatization has been used for different classes of analytes to improve their ionization efficiency, chromatographic separation and chemical stability. This work presents an overview of chemical derivatization methods that have been applied to the quantitative LC-MS/MS analyses of nine classes of molecules, including aldehydes, amino acids, bisphosphonate drugs, carbohydrates, carboxylic acids, nucleosides and their associated analogs, steroids, thiol-containing compounds and vitamin D metabolites, in biological matrices.

Derivatization methods for quantitative bioanalysis by LC–MS/MS

This study was undertaken to measure the radiation exposure level of caregivers following outpatient NaI (I-131) 1,110 MBq therapy for remnant thyroid ablation after total thyroidectomy in patients with differentiated thyroid cancer, and to evaluate the influence of activities of daily living on radiation exposure level, with the goal of proposing an optimum method of I-131 therapy. The study included 37 patients with differentiated thyroid cancer, who had undergone total thyroidectomy and received outpatient based remnant thyroid ablation using NaI (I-131) 1,110 MBq, who were satisfying the following requirements: (1) patients who have no evidence of distant metastases, (2) whose living environments were appropriate for outpatient I-131 (1,110 MBq) therapy, and (3) patients who gave written informed consent. The dose rate at a distance of 1 m from the body surface of the patient at the moment of release was measured using survey meters of the GM type or ionization chamber type. The dose level for the caregiver was measured with a personal dosimeter in all cases. The dose rate at a distance of 1 m from the patient’s body surface 1 h after I-131 administration was in the range of 29–115 μSv/h (mean 63.8 μSv/h). The 7-day cumulative effective dose of caregivers was 0.11 ± 0.08 mSv, on an average, in 34 dosimeters. In 31 of 34 dosimeters, cumulative effective dose of caregivers was below 0.2 mSv. Dose levels exceeding 0.2 mSv were recorded in 3 cases (0.21, 0.35 and 0.43 mSv in one case each). These results suggest that the exposure level of family members (caregiver and others) was minimal and is lower than the radiation levels affecting human environments. Outpatient-based remnant thyroid ablation with I-131 (1,110 MBq) performed after total thyroidectomy in patients with differentiated thyroid cancer is safe if applied in accordance with the appropriate supervision and guidance by experts with certain qualifications.

Thyroid remnant ablation using 1,110 MBq of I-131 after total thyroidectomy: regulatory considerations on release of patients after unsealed radioiodine therapy.

A method for the quantification of progesterone (PROG) in human saliva using liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) has been developed and validated. The saliva was deproteinized with acetonitrile, purified using a Strata™-X cartridge, and subjected to LC-ESI-MS/MS. Quantification was based on selected reaction monitoring, and deuterated PROG was used as the internal standard. This method allowed the reproducible (intra- and inter-assay relative standard deviations, <2.2%) and accurate (analytical recovery, 96.6-99.7%) quantification of the salivary PROG using a 400 μL sample, and the limit of quantification was 12.5 pg/mL. The developed method enabled detection of the variation in the salivary PROG concentrations of healthy volunteers during the menstrual cycle and measurement of the salivary concentrations of pregnant women. The method is expected to be an alternative to the blood PROG monitoring in clinical examinations, because saliva collection is easy, non-invasive and repeatable.

Development and validation of stable‐isotope dilution liquid chromatography–tandem mass spectrometric method for determination of salivary progesterone

Salivary chenodeoxycholic acid and its glycine-conjugate: Their determination method using LC-MS/MS and variation of their concentrations with increased saliva flow rate

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Thyroid remnant ablation using 1,110 MBq of I-131 after total thyroidectomy: regulatory considerations on release of patients after unsealed radioiodine therapy.

Development and validation of stable‐isotope dilution liquid chromatography–tandem mass spectrometric method for determination of salivary progesterone

Salivary chenodeoxycholic acid and its glycine-conjugate: Their determination method using LC-MS/MS and variation of their concentrations with increased saliva flow rate