| 引用本文: | 赵明娟,顾霄,郑金琪.16种核苷与核苷酸LC检测方法的建立及质谱裂解规律的研究[J].中国现代应用药学,2022,39(20):2614-2621. |
| ZHAO Mingjuan,GU Xiao,ZHENG Jinqi.Establishment of LC Methods for 16 Nucleosides and Nucleotides and the Study of Cleavage Law by Mass Spectrometry[J].Chin J Mod Appl Pharm(中国现代应用药学),2022,39(20):2614-2621. |
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| 摘要: |
| 目的 建立通用LC-MS法用于分离和鉴定核苷(酸)化合物。方法 选用ODS-AQ柱，流动相A为缓冲液1(120mmol·L-1 Na2HPO4，120mmol·L-1 KH2PO4和3mmol·L-1 TBAOH)，流动相B为水，流动相C为甲醇，梯度洗脱，对16种核苷和核苷酸化合物进行分离分析。采用电喷雾离子化(ESI)检测，喷雾电压4000V(正离子模式)/3500V(负离子模式)，雾化气压力45psi，干燥气流量10L·min-1，去溶剂温度350℃。碎裂电压为180V，碰撞能量设置为5~30eV，对4种不同类型的核苷和核苷酸化合物的质谱碎片进行分析。结果 建立的LC方法对16个代表性核苷(酸)化合物达到了基线分离(R>2.0)，基于质谱碎片规律，构建核苷(酸)化合物的质谱平台。结论 建立的LC-MS方法可为未知的核苷(酸)化合物的分离与鉴定提供参考。 |
| 关键词: 液相色谱-质谱 核苷(酸)化合物 基线分离 质谱平台 |
| DOI：10.13748/j.cnki.issn1007-7693.2022.20.007 |
| 分类号:R917 |
| 基金项目:浙江省基础公益研究计划(LGF19H300001) |
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| Establishment of LC Methods for 16 Nucleosides and Nucleotides and the Study of Cleavage Law by Mass Spectrometry |
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ZHAO Mingjuan1, GU Xiao2, ZHENG Jinqi2
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1.Hangzhou Zhongmeihuadong Pharmaceutical Co., Ltd., Hangzhou 310015, China;2.Zhejiang Institute for Food and Drug Control, Key Laboratory of Drug Contacting Materials Quality Control of Zhejiang Provincial, Key Laboratory for Core Technology of Generic Drug Evaluation National Medical Product Administration, Hangzhou 310052, China
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| Abstract: |
| OBJECTIVE To establish a general LC-MS method for the separation and identification of nucleoside and nucleotide compounds.METHODS The ODS-AQ column was picked, the mobile phase A was buffer 1(120 mmol·L-1 Na2HPO4, 120 mmol·L-1 KH2PO4 and 3 mmol·L-1 TBAOH), the mobile phase B was water, and the mobile phase C was methanol, gradient elution. The 16 nucleoside and nucleotide compounds were separated and analyzed. Electrospray ionization (ESI) detection was adopted, spray voltage was 4 000 V (positive ion mode)/3 500 V(negative ion mode), atomizing gas pressure was 45 psi, drying gas flow rate was 10 L·min-1, and solvent removal temperature was 350 ℃. The fragmentation voltage was 180 V, and the collision energy was set to 5-30 eV. Mass spectrometry fragments of 4 different types of nucleoside and nucleotide compounds were analyzed.RESULTS The established LC method achieved baseline separation(R>2.0) for 16 representative nucleoside and nucleotide compounds. Based on the mass spectrum fragmentation rule, a mass spectrometry platform for nucleoside and nucleotide compounds was constructed.CONCLUSION The established LC-MS method can provide reference for the separation and identification of unknown nucleoside and nucleotide compounds. |
| Key words: LC-MS nucleosides and nucleotides compounds baseline separation mass spectrometry platform |
