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To establish an HPLC method for determination of related substances and purity in pregabalin API.
The analytical column was an Inertsil ODS-3 (150 mm×4.0 mm，3 μm)，the mobile phase A was buffer (7.05 g ammonium dihydrogen phosphate and 1.45 g diammonium hydrogen phosphate dissolved in 1 000 mL water)-methanol-acetonitrile(900：80：20) and the mobile phase B was acetonitrile，the whole carried out by gradient elution at a flow rate of 0.8 mL·min-1，the detection wavelength was set at 210 nm，the column temperature was 30 ℃ and the injection volume was 50 μL.
Pregabalin was separated completely from the impurities and degradation products (the resolution>2.0). The test solution was stable for at least 48 h. The LOQs of other impurities (verification was performed by using pregabalin)，lactam，4-alkene pregabalin，5-alkene pregabalin，trimer，3-isobutylglutaric acid (PGB-3)，3-isobutyl glutaric acid monoamide (PGB-5)，R-phenethylamine，4-isobutyl-2，6-piperidinedione (PGB-5B)，monoamide phenylethylamine (PGB-5C) and phenylethylamine adipate (PGB-5D) were 0.05%，0.01%，0.01%，0.03%，0.01%，0.05%，0.03%，0.01%，0.01%，0.01% and 0.01%. The linear correlation coefficients of other impurities (verification was performed by using pregabalin)，lactam，4-alkene pregabalin，5-alkene pregabalin，trimer，PGB-3 and PGB-5 were all more than 0.99. The linear ranges were LOQ-150% of impurities’ specification，respectively. The average recoveries (n=9) of lactam，4-alkene pregabalin，5-alkene pregabalin，trimer，PGB-3 and PGB-5 were 100.6% (RSD=0.56%)，100.2% (RSD=0.38%)，100.5% (RSD=0.46%)，101.1% (RSD=1.1%)，100.0% (RSD=0.63%)，100.0% (RSD=0.54%). The repeatability and intermediate precision completely met the requirements. The impurities contents in three batches of pregabalin API 6 months accelerate and 60 months long-term stability test completely met the requirements，respectively.
This method is simple，rapid，sensitive and specific to be used for the determination of related substances and purity in phenethylamine process pregabalin API.
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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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