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To establish a method for the determination of 18 phthalates (PAEs) metabolites in urine by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) based on solid-phase support liquid-liquid extraction (SLE) technology.
Urine sample spiked with internal standards was first hydrolyzed by enzyme, then purified on a SLE column. The separation was performed on a BEH C18 column. The detection was performed in multi-reaction monitoring scan under negative mode. Internal standard method was applied for quantitative analysis.
The 18 PAEs metabolites showed good linear relationships in the range of 0.10-80 ng/ml (r>0.999). The average recoveries of 18 PAEs metabolites ranged from 84.0%-113.0% with relative standard deviations between 1.1% and 9.5%. The limits of detection and quantitation of the method were 0.001-0.07ng/ml and 0.002-0.2 ng/ml, respectively. The intra-day and the inter-day precisions were 1.3%-7.0% and 1.0%-8.1%, respectively. 160 urine samples were analyzed with this method. Except for 3 PAEs metabolites that were not detected, the detection rates of the remaining 15 PAEs metabolites ranged from 1.9% to 100%, and the detection rates of 8 PAEs metabolites were 100%. Among them, mono-n-butyl phthalate had the highest concentrations with a median concentration of 126 ng/ml.
This method is simple, sensitive, and accurate, and it is suitable for the determination of 18 PAEs metabolites in large batchs of urine samples.
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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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