顶空气相色谱法测定注射用利福霉素钠中的残留溶剂

Determination of residual organic solvents in Rifamycin sodium for injection by headspace gas chromatography

目的采用顶空气相色谱法测定注射用利福霉素钠中的残留溶剂。方法采用DB—FFAP毛细管柱（30m×0．32mm，0．25μm），柱温采用程序升温：40℃保持5min，以10℃·min。升至50cC保持1min，再以50℃·min-1升至200℃保持5min，进样口温度200℃，FID检测器温度250℃，分流比20：1，N，流速0．7mL·min-1。结果3种残留溶剂各峰的分离度良好，异丙醇、乙醇、乙酸丁酯顶空进样检测的色谱峰面积与浓度的线性关系良好，线性范围分别为0．0100～4．0128（r=0．9999）、0．0100～4．0141（r=0．9999）、9．9×10～3．9766mg·mL-1（r=0．9999）；最低检测限分别为0．9910、1．1968、1．3996μg·mL-1；平均加样回收率为97．9％～103．4％，RSO为0．9％～1．9％（n=3）。结论所用方法选择性强、重复性好、灵敏度高、操作方便，可作为注射用利福霉素钠中残留溶剂的质控方法。

OBJECTIVE To establish a headspace GC method for the content determination of the residual organic solvents in Rifa- mycin sodium for injection. METHODS The determination were performed on a DB - FFAP （30 m - 0.32 mm,0.25 μm） capillary column, using temperature programming. The initial temperature was kept at 40 h2 for 5 min, then the temperature was raised to 50℃ at the rate of 10 ℃ .rain -j and kept for 1 rain. At last the temperature was raised to 200 ℃ at the rate of 50% .min-1 and kept for 5 min. FID was used as detector with a temperature of 250 ℃. The inlet temperature was 200 ℃, and the split ratio was 20 ： 1. RESULTS All the peaks were completely separated. The method had good linearity with a range of 0.0100 -4. 0128 mg mL-1 for isopropyl alcohol （ r = 0. 9999 ）, 0. 0100 - 4. 0141 mg mL-1 for ethanol （ r = 0. 9999 ） , and 9.9 x 10 -3 - 3. 9766 mg. mL- 1 for butyl acetate （ r = 0. 9999）. The detection limits of them were 0. 9910 μg mL-1 , 1. 1968μg mL-1 and 1. 3996 μg mL-1 , respectively. The average recoveries were in the range of 97.9% - 103.4% with RSD of 0.9% - 1.9% （ n = 3 ）. CONCLUSION The method is selective, repeatable, sensitive and convenient, and can be used to control the residual organic solvents in Rifamycin sodium for injection.