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目的采用高效液相色谱法检测破伤风抗毒素注射液中苯酚残留量,并对方法进行验证及初步应用。方法色谱柱:C18色谱柱;流动相:甲醇-超纯水(体积比1∶1);流速:0.5 ml/min;检测波长:270 nm;柱温:35℃;进样量:5μl。对方法进行专属性、线性、检测限、准确性、精密性验证。用验证后的方法检测4批破伤风抗毒素注射液的苯酚残留量。结果供试品溶液中加入60μg/ml的苯酚对照品溶液和间甲酚对照品溶液的平均回收率为99.92%,相对标准偏差(relative standard deviation,RSD)为0.139 3%;在1~60μg/ml范围内,苯酚对照品色谱峰面积与浓度呈良好的线性关系,回归方程:Y=9.869 19 X+1.082 34 e-1,r=0.999 96;按照信噪比(S/N)≥3确定最低检测限为0.05μg/ml;供试品溶液中加入不同浓度苯酚对照品溶液的平均回收率分别为101.75%和97.03%,RSD分别为0.025%和0.796%;供试品溶液5次检测结果的RSD为1.485 9%。4批破伤风抗毒素注射液中的苯酚残留量均符合《中国药典》三部(2010版)≤890μg/ml的要求。结论高效液相色谱法检测破伤风抗毒素注射液中苯酚残留量快速、简便,且专属性、线性、准确性、精密性良好。
OBJECTIVE To determine the amount of phenol residues in tetanus antitoxin injection by high performance liquid chromatography (HPLC) and verify the method and preliminary application. Methods Column: C18 column; mobile phase: methanol - ultrapure water (volume ratio 1: 1); flow rate: 0.5 ml / min; detection wavelength: 270 nm; column temperature: 35 ℃; The method of specificity, linearity, detection limits, accuracy, precision verification. The phenol residue of 4 batches of tetanus antitoxin injection was tested by the validated method. Results The average recovery of the 60μg / ml phenol reference solution and the m-cresol reference solution was 99.92%, the relative standard deviation (RSD) was 0.139 3% ml, the linear regression equation of the chromatographic peak area of phenol reference substance was: Y = 9.869 19 X + 1.082 34 e-1, r = 0.999 96, which was determined according to the signal to noise ratio (S / N) ≥3 The lowest detection limit was 0.05μg / ml. The average recoveries of the reference solutions with different concentrations of phenol were 101.75% and 97.03%, respectively, and the RSDs were 0.025% and 0.796% respectively. The test results of the test solution The RSD is 1.485 9%. The residues of phenol in 4 batches of tetanus antitoxin injection met the requirements of the Chinese Pharmacopoeia (2010 edition) ≤890 μg / ml. Conclusion The HPLC method for the determination of tetracycline antitoxin injection phenol residue fast, simple, and specificity, linearity, accuracy, precision and good.