HPLC法同時測定重酒石酸去甲腎上腺素注射液和鹽酸去氧腎上腺素注射液的含量及有關物質

摘 要 目的：建立測定重酒石酸去甲腎上腺素注射液和鹽酸去氧腎上腺素注射液含量及有關物質的方法。方法：采用高效液相色譜法，色譜柱：Kromasil C18色譜柱(4.6 mm×250 mm，5 micro;m)；流動相：甲醇-乙腈-庚烷磺酸鈉溶液（1∶1∶8）；檢測波長：280 nm；流速：1 ml/min；柱溫：30 ℃。結果：重酒石酸去甲腎上腺素在80～320 μg/ml范圍內與峰面積呈良好的線性關系，r=0.999 8；高、中、低3種濃度的平均回收率為101.2%，RSD為0.18%(n=9)。重酒石酸去甲腎上腺素的最小檢測限為152.3 ng/ml。鹽酸去氧腎上腺素在100～400 μg/ml范圍內與峰面積呈良好的線性關系，r=0.999 6；高、中、低3種濃度的平均回收率為98.1%，RSD為0.051%(n=9)。鹽酸去氧腎上腺素的最小檢測限為103.8 ng/ml。結論：該法簡便、準確、靈敏度高，重現性好，可用于重酒石酸去甲腎上腺素注射液和鹽酸去氧腎上腺素注射液的含量測定和有關物質檢查。

關鍵詞 高效液相色譜法 重酒石酸去甲腎上腺素 鹽酸去氧腎上腺素 注射液 含量測定 有關物質

中圖分類號：O657.72；R927.2 文獻標識碼：A 文章編號：1006-1533(2012)07-0038-04

Simultaneous determination of both norepinephrine bitartrate injection and phenylephrine hydrochloride injection and their related substances by HPLC method

SUN Ke-gang， SHI Jian-guo， JIANG Yu-dan

(Shanghai Harvest Pharmaceutical Co.， Ltd， Shanghai， 201206)

ABSTRACT Objective: To establish a methods for the determination of both norepinephrine bitartrate injection and phenylephrine hydrochloride injection and their related substances. Methods: An HPLC was performed on a column of Kromasil C18 (250 mm×4.6 mm，5 μm) with the mobile phase of methanol - acetonitrile - sodium heptane solution (1：1：8) at detection wavelength of 280 nm， flow rate of 1.0 ml/min and column temperature of 30 ℃. Results: For norepinephrine bitartrate， the calibration curve was linear (r=0.999 8) over the range of 80～320 μg/ml， the average recovery was 101.2% with RSD 0.18% and the limit of detection was 152.3 ng/ml. For phenylephrine hydrochloride， the calibration curve was linear (r=0.999 6) over the range of 100～400 μg/ml， the average recovery was 98.1% with RSD 0.051% and the limit of detection was 103.8 ng/ml. Conclusion: This method is simple， accurate， sensitive and good reproducible， which can be applied in the determination of both norepinephrine bitartrate injection and phenylephrine hydrochloride injection and their related substances.

KEY WORDS HPLC； norepinephrine bitartrate ；phenylephrine hydrochloride； injection；assay； related substances

重酒石酸去甲腎上腺素和鹽酸去氧腎上腺素均為腎上腺素受體激動藥，具有收縮血管的作用。臨床上用于治療休克及維持血壓。重酒石酸去甲腎上腺素注射液[1]和鹽酸去氧腎上腺素注射液[2]均為《中國藥典》2010年版二部收載品種。重酒石酸去甲腎上腺素注射液的含量和有關物質測定均為高效液相色譜法，但色譜條件不同，鹽酸去氧腎上腺素注射液含量測定方法采用溴量法，有關物質測定采用薄層色譜法。故將兩種注射液的含量測定及有關物質測定方法進行統一，以方便生產檢驗。……