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To develop a liquid-liquid extraction combined with ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry (LLE-UHPLC-MS/MS) method for simultaneous determination of nine monoester phthalate metabolites (mPAEs) in urine.
1 ml urine sample was subjected to enzymatic hydrolysis by the addition of ammonium acetate solution and β-glucuronidase at 37 °C on a shaker for 16 h. Subsequently, 20 μl of formic acid was added and thoroughly mixed. Liquid-liquid extraction was performed with 3 ml of ethyl acetate, then the mixture was centrifuged and the supernatant was concentrated under nitrogen flow. The residue was reconstituted with 0.20 ml of acetonitrile-water solution (50∶50, v/v). Chromatographic separation was performed on a BEH C18 column (2.1 mm×100 mm, 1.7 μm) using a mobile phase of 0.10% acetic acid in acetonitrile and 0.10% aqueous acetic acid. Analytes were ionized via electrospray ionization (ESI) in negative ion mode and detected by multiple reaction monitoring (MRM), and quantification was achieved through the internal standard curves.
Good linear relationship was obtained for the analytes within 0.50 to 200 ng/ml, with correlation coefficients greater than 0.999. When 1 ml of urine sample was utilized for analysis, the detection limits and the quantitation limits of the method were 1.5×10-3 to 0.29 ng/ml and 4.9×10-3 to 0.98 ng/ml, respectively. The recovery rates of the method ranged from 87.05% to 111.5%, with intra-day relative standard deviations of 0.31% to 3.05%, and inter-day relative standard deviations of 0.59% to 3.46%. The nine monophthalates in 277 urine samples from healthy individuals were determined by the proposed method. Except for mono-benzyl phthalate (MBzP), which had a detection rate of 87.73%, the detection rates of other monophthalates were 100%. Mono-butyl phthalate (MnBP) had the highest median concentration of 194.10 μg/g creatinine, while MBzP had the lowest median concentration of 3.7×10-2 μg/g creatinine.
The established method for simultaneous determination of 9 monophthalates in urine samples was simple, sensitive, and accurate, which is suitable for the accurate exposure assessment of these substances in urine.
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| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |
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