Optimization of a NH4PF6-enhanced, non-organic solvent, dual microextraction method for determination of phthalate metabolites in urine by high performance liquid chromatography

Wu, Jia; Ye, Zhihan; Li, Xiaolong; Wang, Xuedong; Luo, Fangjun; Sheng, Bo; Li, Yiwei; Lyu, Jianxin

doi:10.1016/j.jchromb.2016.01.024

Cited by 13 publications

(2 citation statements)

References 32 publications

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“…A Sepex GP-C18 column (1.8 mm, 2.1 mm ∅ × 100 mm) was used for chromatographic separation of phthalates. The mobile phase consisted of acetonitrile-acetic acid (99.9/0.1, v/v) and water, which were designated as A and B, respectively [30]. The gradient elution program was as follows: from 0 to 5 min, 30% A; linear increase to 90% A, from 5 to 7 min; linear decrease to 30% A; and, stabilization at initial condition (30% A, 70% B) for 3 min.…”

Section: Analysis Of Phthalatesmentioning

confidence: 99%

Phthalate exposure in Thai children and adolescents

et al. 2017

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BackgroundPhthalates are found in products made of plastic. Because of concerns regarding the hazards of phthalate exposure, including endocrine disruption, many countries have regulations to restrict their use in products used by children. However, in Thailand, no such restrictions exist, and data relating to phthalate exposure are scarce.ObjectivesTo determine the level of exposure of Thai children and adolescents to phthalates, and study its associations with sociodemographic data and the exposure to potential sources of phthalates.MethodsHealthy children aged 2–18 y were enrolled into the present cross-sectional study between January 2016 and December 2016 inclusive. Their anthropometric indices and Tanner staging were determined. Urinary concentrations of the phthalate metabolites, monomethyl phthalate (MMP) and mono-n-butyl phthalate (MBP), were determined in spot samples by high-performance liquid chromatography to estimate the level of phthalate exposure. Associations between sociodemographic data, exposure to potential sources of phthalates, and phthalate metabolite concentrations were analyzed.ResultsWe included 103 boys and 118 girls with a mean age of 9.4 ± 3.64 (range 2.8–17.1) y and detected MMP in 28.5% and MBP in 88.6%. The geometric means (interquartile range) of urinary MMP and MBP were 3400 (2489, 4642) and 214.4 (164, 279) μg/g creatinine (Cr), respectively. Significant associations were found between exposure to floor cleaning products and Cr-adjusted urinary MMP level (P< 0.05), and paint and Cr-adjusted urinary MMP and MBP levels (P< 0.05). Prepuberty was significantly associated with urinary Cr-adjusted MMP level.ConclusionUrinary phthalate metabolite levels were high in a proportion of Thai children and adolescents. Exposure to floor cleaning products and paint is associated with phthalate exposure, and advanced Tanner stage is negatively associated with urinary Cr-adjusted MBP.

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Section: Analysis Of Phthalatesmentioning

confidence: 99%

Phthalate exposure in Thai children and adolescents

et al. 2017

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“…To overcome these issues, the development of microextraction techniques has been proposed [11][12][13], starting with solidphase microextraction (SPME) [14]. For the pretreatment of samples for the analysis of PAs and their metabolites, SPE is commonly used [8], although other techniques have also been explored, such as LLE [15], magnetic solid phase extraction (MSPE) using magnetic carbon nanotubes [16], dispersive liquid-liquid microextraction (DLLME) [17,18], hollow fiber liquid-phase microextraction (HF-LPME) [19], and SPME [20,21]. However, direct analysis of urine samples has also been proposed [22].…”

Section: Introductionmentioning

confidence: 99%

Disposable Pipette Extraction (DPX) Coupled to HPLC-DAD as an Alternative for the Determination of Phthalic Monoesters in Urine Samples

Comelli¹,

Will²,

Morés³

et al. 2022

Separations

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Phthalates are widely used in industry, but adverse effects on human health have been reported due to exposure to these chemicals. In the human body, they are metabolized into phthalic monoesters, which are used to monitor human exposure and assess risk. Urine is one of the main biological samples used, due to its easy access and collection, and also being the main elimination pathway for phthalates. Urine samples are complex; therefore, sample preparation is a critical step. Disposable pipette extraction (DPX) has not previously been reported for quantifying phthalates in urine and is here presented as a fast and low sample consumption method. A fully optimized RP-DPX method was developed for determination of free monomethyl phthalate, monobutyl phthalate, monobenzyl phthalate, and monoethylhexyl phthalate from urine samples. Analytical parameters of merit were obtained. The values of R2 were ≥0.9832, and the LOD and LOQ varied from 3.0 to 7.6 μg L−1 and 10 to 25 μg L−1, respectively. Intraday (n = 3) and interday (n = 9) precision were ≤13.6 and 15.6%. The accuracy, as relative recovery, presented a range from 83 to 120%. The method was robust after performing the Youden test. Compared to other methods, this work stands out due to its short extraction time and sample consumption.

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A rapid method for the quantification of urinary phthalate monoesters: A new strategy for the assessment of the exposure to phthalate ester by solid‐phase microextraction with gas chromatography and tandem mass spectrometry

Elliani

Naccarato

Malacaria

et al. 2020

J of Separation Science

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In the following work, a new method for the analysis of the phthalate monoesters in human urine was reported. Phthalate monoesters are metabolites generated as a result of phthalate exposure. In compliance with the dictates of Green Analytical Chemistry, a rapid and simple protocol was developed and optimized for the quantification of phthalate monoesters (i.e., monoethyl phthalate, monoisobutyl phthalate, mono‐n‐butyl phthalate, mono‐(2‐ethylhexyl) phthalate, mono‐n‐octyl phthalate, monocyclohexyl phthalate, mono‐isononyl phthalate) in human urine, which entails preceding derivatization with methyl chloroformate combined with the use of commercial solid phase microextraction and the analysis by gas chromatography‐triple quadrupole mass spectrometry. The affinity of the derivatized analytes toward five commercial coatings was evaluated, and in terms of analyte extraction, the best results were reached with the use of the divinylbenzene/carboxen/polydimethylsiloxane fiber. The multivariate approach of experimental design was used to seek for the best working conditions of the derivatization reaction and the solid phase microextraction, thus obtaining the optimum response values. The proposed method was validated according to the guidelines issued by the Food and Drug Administration achieving satisfactory values in terms of linearity, sensitivity, matrix effect, intra‐ and inter‐day accuracy, and precision.

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Optimization of a NH4PF6-enhanced, non-organic solvent, dual microextraction method for determination of phthalate metabolites in urine by high performance liquid chromatography

Cited by 13 publications

References 32 publications

Phthalate exposure in Thai children and adolescents

Phthalate exposure in Thai children and adolescents

Disposable Pipette Extraction (DPX) Coupled to HPLC-DAD as an Alternative for the Determination of Phthalic Monoesters in Urine Samples

A rapid method for the quantification of urinary phthalate monoesters: A new strategy for the assessment of the exposure to phthalate ester by solid‐phase microextraction with gas chromatography and tandem mass spectrometry

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