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目的建立高效液相色谱法同时测定氯霉素甲硝唑洗鼻剂中氯霉素、甲硝唑含量及氯霉素分解产物氯霉素二醇物、对硝基苯甲醛的检测方法。方法采用高效液相色谱法。Intersil C18分析色谱柱(4.6 mmID×250 mm,粒径5μm);流动相:甲醇-水-三乙胺(480∶520∶7,含1%磷酸二氢钠,0.2%庚烷磺酸钠,磷酸调pH值为3.0);流速1.0 ml/min;检测波长270 nm。结果甲硝唑、氯霉素二醇物、氯霉素和对硝基苯甲醛的理论板数分别为4700、4500、4400、1500。回归方程分别为:y=424 145.7+19 156 100.5 X(r=0.9999),y=39817070.9x+1373589.3(r=0.9998),y=65390024.2 x-5660.6(r=0.9999),y=83051977.5 x-284191.7(r=0.9998);线性范围分别为0.4230~2.115μg,0.4500~2.250μg,0.0330~0.1650μg,0.02220~0.1110μg;平均回收率(±RSD)分别为99.5%(±1.4),98.7%(±1.3),102.3%(±1.8%),96.3%(±1.9);最低检出限分别约为0.0002μg,0.0002μg,0.0002μg和0.003μg。结论用高效液相色谱法同时测定氯霉素甲硝唑洗鼻剂中甲硝唑、氯霉素二醇物、氯霉素、对硝基苯甲醛的含量,操作简便,结果准确。
OBJECTIVE To establish a HPLC method for the simultaneous determination of chloramphenicol and metronidazole in chloramphenicol metronidazole nasal drops and detection of chloramphenicol diol and p-nitrobenzaldehyde. Methods Using high performance liquid chromatography. (4.6 mmID × 250 mm, particle size 5 μm); mobile phase: methanol-water-triethylamine (480: 520: 7 containing 1% sodium dihydrogen phosphate, 0.2% sodium heptane sulfonate, Phosphoric acid adjusted to pH 3.0); flow rate 1.0 ml / min; detection wavelength 270 nm. Results Metronidazole, chloramphenicol diol, chloramphenicol and p-nitrobenzaldehyde theoretical plates were 4700,4500,4400,1500. The regression equations were: y = 424 145.7 + 19 156 100.5 X (r = 0.9999), y = 39817070.9x + 1373589.3 (r = 0.9998), y = 65390024.2 x- 5660.6 (r = 0.9999), y = 83051977.5 x-284191.7 (r = 0.9998). The linear range was 0.4230 ~ 2.115μg, 0.4500 ~ 2.250μg, 0.0330 ~ 0.1650μg and 0.02220 ~ 0.1110μg respectively.The average recovery was ± 0.5% 1.3), 102.3% (± 1.8%) and 96.3% (± 1.9), respectively. The detection limits were 0.0002μg, 0.0002μg, 0.0002μg and 0.003μg respectively. Conclusions Simultaneous determination of metronidazole, chloramphenicol diol, chloramphenicol and p-nitrobenzaldehyde in chloramphenicol metronidazole nasal drops by high performance liquid chromatography has the advantages of simple and convenient operation and accurate results.