Table 3.
Literature examples of analytical methodologies with their basic validation data used for the determination of monophthalates by LC and GC techniques.
| Analytes | Matrix | Sample preparation technique | Final determination technique | Injected volume [μL] | Linearity range [μg/L] | Coefficient of determination R2 | Precision of the method | References | |||
|---|---|---|---|---|---|---|---|---|---|---|---|
| Recovery [%] | CV [%] | LOD [μg/L] | LOQ [μg/L] | ||||||||
| MEP, MnBP, MEHP, MEHHP | Urine | SPE after enzymatic hydrolysis (β-glucuronidase) | HPLC-MS/MS | 20 | 10–500 | 0.9869–0.9928 | 95.2–100.7 | 1.8–6.0 | 0.05–3 | 0.5–8 | Mankidy et al., 2013 |
| MEP, MBzP, MiBP, MnBP, MEHP, 5OH-MEHP, 5oxo-MEHP | Urine | SPE after enzymatic hydrolysis (β-glucuronidase) | UPLC-MS/MS | 10 | 1–250 | 0.9950 | 97–104 | 7–12 | – | 0.1–0.5 | Servaes et al., 2013 |
| MEP, MnBP, MBzP, MEHP, 5OH-MEHP, 5oxo-MEHP, MOP | Urine | LLE after enzymatic hydrolysis (β-glucuronidase) | HPLC-MS/MS | 600 | 0.4–2,000 | 0.9900 | 84.6–106 | 2.5–8.3 | 0.25–1.0 | 0.5–2.0 | Koch et al., 2003 |
| MMP, MEP, MnBP, MBzP, MEHP, MOP | Urine | SPE after enzymatic hydrolysis (β-glucuronidase) | UPLC-MS/MS | 200 | 1.0–1,000 | 0.9950 | 82.5–118.4 | 2.2–11.3 | 0.3–0.5 | 1.0–1.5 | Xu et al., 2016 |
| MEP, MnBP, MEHP, MBzP | Urine | SPE after enzymatic hydrolysis (β-glucuronidase) | HPLC-MS/MS | 20 | 5–2,000 | 0.9968–0.9993 | 81.8–125.3 | 0.07–10.2 | 0.85–5.33 | 2.8–17.8 | Cheng et al., 2014 |
| MEHP, MEHHP, MEOHP, 5cx-MEPP, 2cx-MMHP | Urine | LLE after enzymatic hydrolysis (β-glucuronidase) | UPLC-MS/MS | 5 | 0.5–100 | 0.9900 | 90.2–102.0 | 0.9–12.0 | – | 1.2–2.6 | Monfort et al., 2012 |
| MEP, MiBP, MnBP, MBzP, MiNP, MEHP, MEOHP, MEHHP | Urine | LLE after enzymatic hydrolysis (β-glucuronidase) + derivatization (BSTFA with 1% of TMCS) | GC-MS | 2 | 0.05–100 | 0.9923–0.9991 | 61.6–100.1 | 2.1–16.3 | 0.05–0.2 | 0.1–0.5 | Kim et al., 2014 |
| MnBP, MiBP, MBzP, MEHP, MEOHP, MECPP, MCPP | Urine | LLE after enzymatic hydrolysis (β-glucuronidase/ arylsulphatase) + derivatization (MTBSTFA) | GC-MS | 1 | – | >0.995 | 86.2–136.2 | 8.6–31.7 | 5 | – | Bamai et al., 2015 |
| MMP, MEP, MnBP, MEHP | Environmental waters, urine | SPME on-fiber derivatization (diazomethane) after enzymatic hydrolysis (β-glucuronidase) | GC-MS | 0 (solventless technique) | 0.1–150 | 0.989–0.995 | – | 14–16 | 0.1–4.4 | 0.3–8.6 | Alzaga et al., 2003 |
| MiBP, MOP, MMP, MnBP, MCHP, MEHP, MiNP, MBzP | Urine | HF-LPME after enzymatic hydrolysis (β-glucuronidase) with derivatization (BSTFA) | GC-MS | not given | 5–1000 | 0.9747–0.9961 | – | 12–20 | 0.77–23 | 1.2–39 | Moreira Fernandeza and André, 2017 |
| MMP, MEP, MnBP, MEHP | Standard solutions | No extraction and derivatization | GC-MS | 2 | 43.5–50000 | 0.9817–0.9993 | – | 5.1–9.1 | 14.5–24.5 | 43.5–75 | Proposed method |
MMP, monomethyl phthalate; MEP, monoethyl phthalate; MnBP, mono-n-butyl phthalate; MBzP, monobenzyl phthalate; MEHP, mono-(2-ethylhexyl) phthalate; MOP, mono-n-octyl phthalate; MiNP, mono-isononyl phthalate; MEHHP, mono-(2-ethyl-5-hydroxyhexyl) phthalate; MEOHP, mono-(2-ethyl-5-oxohexyl) phthalate; 5cx-MEPP/MECPP, mono-(2-ethyl-5-carboxypentyl) phthalate; 2cx-MMHP, mono-(2-carboxymethylhexyl) phthalate; 5OH-MEHP, 5-Hydroxy-mono-(2-ethylhexyl) phthalate; 5oxo-MEHP, 5-oxo-mono-(2-ethylhexyl) phthalate; MCPP, mono-(3-carboxypropyl) phthalate; MCHP, mono-cyclohexyl phthalate; BSTFA, N,O-bis(trimethylsilyl)-trifluoroacetamide; TMCS, trimethyl chlorosilane; MTBSTFA, N-methyl-N-(tert-butyldimethylsilyl)-trifluoroacetamide; SPE, Solid-Phase Extraction; LLE, Liquid-Liquid Extraction; SPME, Solid-Phase Microextraction; HF-LPME, Hollow Fiber Liquid Phase Microextraction; CV, coefficient of variability; LOD, limit of detection; LOQ, limit of quantification.