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To establish a method for the determination of 17 kinds of anti-allergic compounds in medical cold compress by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry（SPE-UPLC-MS/MS）. Common medical cold compress matrices were suitable for this new method.
Three pretreatment methods were compared：prime pass-through column purification，SPE purification including HLB and MCX solid-phase extraction. The pretreatment was optimized by focusing on the kind of solid-phase extraction，the type and volume of elution solvents. The analytes were extracted using methanol and then mixed with water at the ratio of 1:9 in volume，purified with an Agilent Bond Elut HLB column. Waters ACQUITY UPLC BEH C18（100 mm×2.1 mm，1.8 μm）column was used with 0.1% formic acid(with 0.5 mmol·L-1 ammonium acetate)-acetonitrile as mobile phases by gradient elution for separating 17 compounds. Detection was carried out by positive and negative electrospray ionization（ESI）mass spectrometer in multiple reaction monitor (MRM) mode.
All the 17 kinds of compounds showed good linearity in their reasonable ranges（r）>0.99，the limit of detection （LOD） and quantification（LOQ）were 0.01-13.32 μg·g-1 and 0.02-26.64 μg·g-1，respectively. The average recoveries of at three spiked levels were in range of 77.7%-108.5%，with RSDs （n=6） were 0.62%-4.7%. The content range of diclofenac sodium in positive samples was 0.09-27.55 mg per tablet.
The method is simple，sensitive and reliable，and is suitable for determination of 17 illegally add chemical drugs in medical cold compress. Moreover，the method might provide technological support for the detection of illegal additions in medical cold compress.
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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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