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Outline
To develop a liquid chromatography-tandem mass spectrometry method for simultaneous detection of N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA) in irbesartan. APCI (+) MRM mode was selected for detection. Gradient elution was conducted with mobile phase consisting of 0.1% formic acid solution and methanol containing 0.1% formic acid. The method had good specificity. Good linearity was obtained for NDMA and NDEA in the range of 1~120 ng·mL-1 and 0.4~48 ng·mL-1, respectively. The limits of detection (LOD) were 0.5 ng·mL-1 and 0.2 ng·mL-1 for NDMA and NDEA. The relative standard deviation (RSD) of peak area was less than 3.0%. The accuracy was 96.1%~106.2% and repeatability was good. The average percent recovery was 102.5% and 99.9% for NDMA and NDEA, respectively. All samples were stable after being stored for 24 h in auto-injection sampler or at 0 ℃. This method is simple, sensitive and accurate, and can be used for limit test and quantitation of NDMA and NDEA in irbesartan.
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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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