目的 建立同時測定復(fù)方氨基酸注射液（20AA）中焦谷氨酸、醋酸根的HPLC方法。方法 采用GL Sciences Inertsil ODS-3色譜柱（250 mm×4.6 mm，5 μm）；流動相：乙腈–5 mmol/L磷酸溶液（磷酸調(diào)pH 2.5），采用梯度洗脫；檢測波長：210 nm；體積流量：1.0 mL/min；柱溫：25 ℃；進(jìn)樣量：15 μL。結(jié)果 在上述色譜條件下，焦谷氨酸、醋酸根峰與各自相鄰峰的分離度均大于2.0；焦谷氨酸和醋酸根的定量限分別為0.10、0.99 μg/mL，檢測限分別為0.03、0.30 μg/mL；焦谷氨酸和醋酸根分別在0.1～120.0 μg/mL、0.6～540.0 μg/mL與峰面積呈良好的線性關(guān)系。焦谷氨酸和醋酸根的回收率分別為100.04%、98.39%，RSD值分別為0.12%、0.70%。結(jié)論 本方法簡便、靈敏度高、重現(xiàn)性好，適用于復(fù)方氨基酸類制劑中焦谷氨酸和醋酸根的同時檢測。

Objective To establish an HPLC method for simultaneous determination of pyroglutamic acid and acetate ion in Compound Amino Acid Injection (20AA). Methods GL Sciences Inertsil ODS-3 column (250 mm×4.6 mm, 5 μm) was used. The mobile phase consisted of acetonitrile and 5 mmol/L phosphoric acid solution (pH 2.5). The determination was performed by gradient elution. The detection wavelength was set at 210 nm. The flow rate was 1.0 mL/min; the volume of injection was 15 μL, and the temperature of column was set at 25 ℃. Results The resolutions of pyroglutamic acid and acetate ion with their own closely eluting peaks were both good with R > 2.0. The LOQs of pyroglutamic acid and acetate ion were 0.10 and 0.99 μg/mL, respectively. The LODs were 0.03 and 0.30 μg/mL, respectively. Pyroglutamic acid and acetate ion had good linearity in the range of 0.1 — 120.0 μg/mL and 0.6 — 540.0 μg/mL, respectively. The average recoveries were 100.04% and 98.39%, with RSD values of 0.12% and 0.70%, respectively. Conclusion The method is simple and convenient, and has high sensitivity and good reproducibility, and is suitable for the simultaneous determination of pyroglutamic acid and acetate ion in compound amino acid prescriptions.

R927.2

國家自然科學(xué)基金面上項目（31970667）；重大新藥創(chuàng)制國家科技重大專項（2019ZX09721001-006-001）；國家藥典委員會藥品標(biāo)準(zhǔn)制修訂研究課題（2019H03）；天津市“131”創(chuàng)新型人才培養(yǎng)工程項目