首页|超高效液相色谱串联质谱法检测人促红素注射剂中2种抗生素残留

超高效液相色谱串联质谱法检测人促红素注射剂中2种抗生素残留

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目的 建立检测人促红素注射剂中氨苄西林和博来霉素残留的超高效液相色谱串联质谱(UPLC-MS/MS)法.方法 色谱柱为Waters Cortecs T3 柱(100 mm×2.1 mm,2.7 μm);流动相为 0.1%甲酸水溶液-[乙腈-甲醇(95∶5,V/V)],梯度洗脱;流速为0.2 mL/min;柱温为 40℃;进样量为 5 μL.采用电喷雾离子源正离子模式和多反应监测扫描模式.结果 氨苄西林和博来霉素质量浓度分别在 19.38~484.5 ng/mL(r=0.9979,n=5)和 21.26~212.6 ng/mL(r=0.9988,n=5)范围内与峰面积线性关系良好,检测限分别为 0.00969,10.63 ng/mL,定量限分别为 0.0969,21.26 ng/mL;精密度、稳定性试验结果的RSD均小于 4.0%;平均加样回收率分别为 102.11%和 101.77%,RSD为分别为 7.46%和 13.35%;基质效应均不明显(分别为 95.03%和 84.51%).9 家国内生产企业和 1 家国外生产企业的 39 批人促红素注射剂均未检出氨苄西林和博来霉素.结论 所建立的方法操作简单、检测灵敏,结果准确,可用于人促红素注射剂中氨苄西林和博来霉素残留的检测.
Detection of Two Antibiotic Residues in Human Erythropoietin Injection and Human Erythropoietin for Injection by UPLC-MS/MS
Objective To establish an ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for determining the ampicillin and bleomycin residues in Human Erythropoietin Injection and Human Erythropoietin for Injection.Methods The chromatographic column was the Waters Cortecs T3 column(100 mm×2.1 mm,2.7 μm),the mobile phase was 0.1%formic acid aqueous solution-[acetonitrile-methanol(95∶5,V/V)]with gradient elution,the flow rate was 0.2 mL/min,the column temperature was 40℃,and the injection volume was 5 μL.The electron spray ionization with positive ion mode and multiple reaction monitoring mode was adopted.Results The linear ranges of ampicillin and bleomycin were 19.38-484.5 ng/mL(r=0.9979,n=5)and 21.26-212.6 ng/mL(r=0.9988,n=5)respectively.The limits of detection of ampicillin and bleomycin were 0.00969,10.63 ng/mL,respectively,and their limits of quantification were 0.0969,21.26 ng/mL,respectively.The RSDs of precision and stability tests were lower than 4.0%.The average recovery rates of the above two antibiotics were 102.11%and 101.77%,with RSDs of 7.46%and 13.35%respectively.The matrix effects of ampicillin and bleomycin were not obvious,with 95.03%and 84.51%,respectively.No ampicillin or bleomycin was detected in 39 batches of Human Erythropoietin Injection and Human Erythropoietin for Injection from nine domestic manufacturing enterprises and one foreign manufacturing enterprise.Conclusion The established method is simple,sensitive and accurate,which can be used to detect ampicillin and bleomycin residues in Human Erythropoietin Injection and Human Erythropoietin for Injection.

Human Erythropoietin InjectionHuman Erythropoietin for InjectionUPLC-MS/MSampicillinbleomycinresiduecontent determination

唐娜、苏超男、陈统华、肖一桐、王嫦鹤、徐长根

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陕西省食品药品检验研究院,陕西 西安 710065

人促红素注射液 注射用人促红素 超高效液相色谱串联质谱法 氨苄西林 博来霉素 残留 含量测定

2024

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
年,卷(期):2024.33(16)
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