毛细管气相色谱和HPLC法检测头孢美唑中的残留溶剂

Determination of residual organic solvent in cefmetazole by capillary gas chromatography and HPLC

目的建立测定头孢美唑原料药中残留溶剂甲醇、乙醇、二氯甲烷、乙酸乙酯、苯甲醚、N，N-二甲基苯胺的检测方法。方法用Agilent HP-5毛细管气相色谱柱和氢焰离子化检测器，按顶空进样的方式同时测定了头孢美唑中甲醇、乙醇、二氯甲烷、乙酸乙酯、苯甲醚的残留量。用高效液相色谱法，以甲醇-水（75：25）为流动相，检测波长254nm，测定头孢美唑中N,N-二甲基苯胺。结果甲醇、乙醇、二氯甲烷、乙酸乙酯、苯甲醚、N,N-二甲基苯胺的线性范围分别为121．5-607．5μg／mL（r=0．9997，n=5）、199．8～998．9μg／mL（r=0．9998，n=5）、199．5～1247．1μg／mL（r=0．9999，n=5）、15．6-125．2μg／mL（r=0．9993，n=6）、249．5～1247．7μg／mL（r=0．9993，n=5），0．096～0．256μg／mL（r=0．9995，n=5）；3种浓度的平均加样回收率（n=3）为91．34％～104．84％（RSD为1．2％～6．5％1。结论两种检测方法简单，可靠，可以用于头孢美唑原料药的质量控制。

Objective To establish a method for determination of methanol, ethanol, dichloromethane, ethylacetate, methylether and N, N-dimethylaniline in cefmetazole. Methods Five residual organic solvents were determined by using HP-5 as stationary phase, and the samples were injected by head-space sampling mode and analyzed by flame ionization detector. N, N-dimethylaniline was examined by HPLC method, using methanolwater（75 ： 25） as mobile phase and the detection wavelength was 254nm. Results The linear range of six residual organic solvents in cefmetazole were 121.5-607.5μg/mL（r=0.9997, n=5）, 199.8-998.9μg/mL（r=0.9998, n=5）, 199.5-1247.1μg/mL（r=0.9999, n=5）, 15.6-125.2μg/mL（r=0.9993, n=6）, 249.5-1247.7μg/mL（r=0.9993, n=5） and 0.096-0.256μg/mL （r=0.9995, n=5）, respectively. The average recoveries of three levels of concentration were 91.34%-104.84%（RSD at 1.2%-6.5%）. Conclusion Both of the methods are simple, reliable, and can be used to control the quality of cefmetazole.