Full
Outline
To develop a rapid, robust and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for the determination of methylnaltrexone in human plasma.
The plasma samples were pretreated by filtering using solid-phase extraction (SPE) with a weak cation-exchange cartridge. The filtrate samples were separated on an Ultra PFP Propyl column (100 mm×2.1 mm, 5.0 μm) using 20 mmol·L-1 ammonium acetate (containing 1% formic acid) in water-acetonitrile (15∶85, v/v) as mobile phase and methylnaltrexone-d3 as the internal standard (IS). The flow rate was set at 0.4 mL·min-1. Methylnaltrexone and IS were ionized with an ESI source and MRM mode was applied and operated in positive ion mode. The detected ions were m/z 356.3→284.2 and m/z 359.3→287.1, respectively.
The linear range of the developed method was 0.1~120 ng·mL-1, with the lower limit of quantification being 0.1 ng·mL-1. The intra-day and inter-day precisions of the method were less than 7.2% across three validation runs, and the accuracy ranged 94.5%~100.7%. The extraction method using SPE reached a mean recovery of 81.4% for methylnaltrexone, and the mean normalized matrix effect was 99.1%. This method was successfully applied for the pharmacokinetic study of subcutaneous injection of methylnaltrexone bromide in 12 healthy volunteers.
This LC-MS/MS method is proven sensitive, rapid and reproducible, and meets the regulatory requirements of biological analysis.
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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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