聚山梨酯指纹图谱建立及成分鉴定  

Establishment of Fingerprints and Identification Method of Polysorbates

作　　者：王珏[1] 许凯 杨洋 杨锐[1] 孙会敏[1] 肖新月[1] WANG Jue;XU Kai;YANG Yang;YANG Rui;SUN Huimin;XIAO Xinyue(National Institutes for Food and Drug Control·NMPA Key Laboratory for Quality Research and Evaluation of Pharmaceutical Excipients,Beijing,China 100050)

机构地区：[1]中国食品药品检定研究院·国家药品监督管理局药用辅料质量研究与评价重点实验室,北京100050

出　　处：《中国药业》2023年第6期55-60,共6页China Pharmaceuticals

基　　金：国家药典委员会标准提高课题[2021Y27]。

摘　　要：目的 建立聚山梨酯的超高效合相色谱(UPCC)指纹图谱并指认其成分。方法 采用超高效合相色谱质谱联用(UPCC-MS)法。MS条件,离子化模式为ESI^(+);雾化气温度为500℃、流速为800 L/h,源温度为120℃,毛细管电压为2.5 kV,锥孔电压为40 V,采集模式为MS^(E),扫描范围m/z 50~3 000;UPCC条件,色谱柱为ACQUITY UPC^(2)Torus Diol柱(100 mm×3.0 mm,1.7μm),流动相为CO_(2)-甲醇/乙腈(30∶70,V/V),离子化溶剂为甲醇+5 mmol/L甲酸铵(流速为0.2 mL/min),梯度洗脱,流速为1.0 mL/min,柱温为50℃,背压为2 500 psi,进样量为1μL。测定12批不同来源的聚山梨酯80样品及其美国药典(USP)标准品的UPCC图谱,采用中药色谱指纹图谱相似度评价系统(2012.130723版)进行相似度评价,确定共有峰,计算相似度,并指认成分。结果 样品的UPCC图谱有22个共有峰,均指认出具体成分,相似度为0.884~0.966;经验证,样品UPCC图谱与对照指纹图谱一致性较好。结论 建立的UPCC-MS法可快速分离聚山梨酯中的复杂组分,所建UPCC指纹图谱可用于聚山梨酯批间一致性的快速分析。Objective To establish ultra-performance convergence chromatography(UPCC) fingerprints of polysorbates,and to identify its components.Methods UPCC-mass spectrometry(UPCC-MS) was adopted.The MS conditions were as follows:ionization mode was ESI^(+),the atomized gas temperature was 500 ℃,the flow rate was 800 L/h,the source temperature was 120 ℃,the capillary voltage was 2.5 kV,the cone voltage was 40 V,the acquisition mode was MS^(E),and the scanning range was m/z50-3 000.The UPCC conditions were as follows:the chromatographic column was ACQUITY UPC^(2) Torus Diol column(100 mm ×3.0 mm,1.7 μm),the mobile phase was CO_(2)-methanol-acetonitrile(30/70,V/V),and the ionization solvent was methanol+5 mmol/L ammonium formate(0.2 mL/min) with gradient elution,the flow rate was 1.0 mL/min,the column temperature was50 ℃,the backpressure was 2 500 psi,and injection volume was 1 μL.The UPCC chromatograms of 12 batches of polysorbate 80samples from different sources and USP standard samples were determined,and the Similarity Evaluation System for the Chromatographic Fingerprint of Traditional Chinese Medicine(Version 2012.130723) was adopted to determine the common peak,calculate the similarity,and identify the components.Results The UPCC chromatogram of the sample had 22 common peaks,all of which were identified as the specific components,and the similarity was in the range of 0.884-0.966.It was verified that the UPCC fingerprints of the sample were consistent with the reference fingerprint.Conclusion The established UPCC-MS method can rapidly separate the complex components in polysorbates,and the established UPCC fingerprints can be used for rapid analysis of the batch-to-batch consistency of polysorbates.

关 键 词：超高效合相色谱质谱联用法 指纹图谱 聚山梨酯 成分鉴定 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]