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To establish and optimize a rapid direct analysis of real time tandem mass spectrometry (DART-MS/MS) method for the rapid detection of 12 benzodiazepines in blood and urine that can be used in forensic toxicology work.
A DART ion source was used in conjunction with an API4000 Q Trap mass spectrometer. A DART 12Dip-ItTM autosampling module with a module travel speed of 0.6 mm·s-1, a sample volume of 5 μL, and a gate voltage of 200 V were applied. The mass spectrometry section scans in positive ion mode using multiple reaction monitoring (MRM) mode. After further optimization, the DART-MS/MS method was validated and applied to real case samples.
Ethyl acetate was selected as the extractant for liquid-liquid extraction and the temperature of the carrier gas heater was optimized. The method has good selectivity and does not interfere with delayed effects. The linearity was good, and the limits of detection (LODs) for the targets in blood and urine were in the ranges of 0.5-10 ng·mL-1 and 0.2-2 ng·mL-1, respectively. And the limits of quantification (LOQs) were in the ranges of 1-50 ng·mL-1 and 0.5-5 ng·mL-1, respectively. The recoveries ranged from 78.8% to 119%, and the matrix effects ranged from -17.5% to 18.5%. The intra- and inter-day precisions were not greater than 14.4% for the high and intermediate concentrations, and not greater than 18.1% at the limits of quantification. This method enables fast and accurate examination of case samples.
The method is fast and convenient, with good sensitivity, and can be applied to the research and work of rapid detection of toxicants to improve the efficiency of detection.
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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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