摘要
目的确证1批银黄提取物注射液中的非法添加物。方法采用超高效液相色谱法,二极管阵列检测器,ACQUITYUPLC^(TM)T_(3)色谱柱(2.1mm×100mm,1.8μm)为分离柱,柱温:40℃;以乙腈(0.1%磷酸)-水(0.1%磷酸)进行梯度洗脱;流速:0.35 mL/min;进样量:1μL;波长扫描范围190~400 nm,检测波长为276 nm。结果土霉素、双氯芬酸钠的检出限分别是22.4、7.3 mg/mL,色谱保留时间分别为3.7 min、8.3 min左右,多次进样各自的保留时间相差不超过±0.1 min;土霉素在269 nm处有紫外最大吸收,双氯芬酸钠在276 nm处有紫外最大吸收;分离度远大于1.5,满足要求,纯度角和纯度阈值均满足要求,系统适应性良好;对比色谱图保留时间和光谱图的峰形结果,最终确证该批样品中非法添加物为土霉素和双氯芬酸钠。结论本确证方法精准快捷、经济环保,能监管本批次标称为银黄提取物注射液的质量。
Objective To confirm the illegal additives in 1 batch of Yinhuang extract injection. Methods Ultra-performance liquid chromatography was used. Acquity UPLC^(TM)T_(3) column(2.1 mm×100 mm, 1.8 μm) was used as the separation column, the column temperature was 40 ℃. The gradient elution was carried out with acetonitrile(0.1% phosphoric acid) and water(0.1% phosphoric acid). Flow rate was 0.35 mL/min. The sample size was 1 μL. The wavelength scan range is 190-400 nm, the detection wavelength was 276 nm. Results The limits of detection of oxytetracycline and diclofenace sodium were 22.4 and 7.3 mg/mL respectively, and the chromatographic retention time was about 3.7 min, 8.3 min respectively. The retention time difference exceeds ±0.1 min.Oxytetracycline had maximum UV absorption at 269 nm and diclofenace sodium at 276 nm. sparation was greater than 1.5, met the requirements, purity angle and purity threshold meet the requirements, and the system adaptability was good. By comparing the retention time of the chromatogram and the peak shape of the spectrogram, it was confirmed that the illegal additives in the samples were oxytetracycline and diclofenac sodium. Conclusion This confirmative is accurate, fast, economical and environmental friendly, and can monitor the quality of the batch named Yinhuang extract injection.
作者
魏秀丽
张传津
刘道中
张志民
牛华星
李有志
WEI Xiu-Li;ZHANG Chuan-Jin;LIU Dao-Zhong;ZHANG Zhi-Min;NIU Hua-Xing;LI You-Zhi(Shandong Center for Quality Control of Feed and Veterinary Drugs,Shandong Provincial Key Laboratory of Quality Safety Monitoring and Risk Assessment for Animal Products,China Shandong Engineering Laboratory for Drug Resistance Monitoring and Precise Drug Use of Animal Origin Bacteria,Shandong Engineering Laboratory for Chinese Traditional Medicine for Animal,Jinan 250022,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2021年第12期4824-4830,共7页
Journal of Food Safety and Quality
基金
2019年山东省农业重大应用技术创新项目(SD2019XM004)。
关键词
银黄提取物
双氯芬酸钠
土霉素
非法添加
超高效液相色谱-二极管阵列检测器法
Yinhuang extract
diclofenace sodium
oxytetracycline
illegal additive
ultra-performance liquid chromatography-diode array detector method
