{"title":"超高效液相色谱-质谱联用法测定小鼠血液中螺旋皂苷的含量及其在药动学和生物利用度研究中的应用","authors":"Xiaojun Cai, Xiangyi Dai, Zhoupeng Li, Junying Chen, Xianqin Wang, Meiling Zhang","doi":"10.1556/1326.2022.01061","DOIUrl":null,"url":null,"abstract":"\n A simple, rapid, and sensitive method based on UPLC-MS/MS was developed to determine spiraeoside in mouse blood, and was applied to the pharmacokinetics and bioavailability of spiraeoside after mice after intravenous (a dose of 5 mg kg−1) and oral (a dose of 20 mg kg−1) administration. On HSS T3 column set at 40 °C, chromatographic separation was obtained with the mobile phase of acetonitrile and 0.1% formic acid using the gradient elution. Spiraeoside and internal standard (IS) were quantitatively analyzed using multiple reaction monitoring (MRM) mode in electrospray (ESI) positive interface. The MRM mode was monitoring the fragmentation of m/z 465.4→303.1 and m/z 451.3→ 289.2 for spironoside and IS, respectively. The results showed a good linear relationship was in the concentration range of 1–200 ng mL−1 (r > 0.998) and the lower limit of quantification (LLOQ) was 1.0 ng mL−1. The intra- and the inter-day precision (RSD%) of the method was within 14.0%, and the accuracy ranged from 90.0% to 115.0%. The extraction recovery of spriaeoside was better than 63.0%, and the matrix effects were in the range of 86%–98%. It also showed the half-life was short, and the absolute bioavailability was 4.0% in mice. Therefore, the established UPLC-MS/MS method was suitable for the pharmacokinetic and bioavailability study of spiraeoside in mice.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.7000,"publicationDate":"2022-08-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"An UPLC-MS/MS method for quantification of spiraeoside in mouse blood and its application to a pharmacokinetic and bioavailability study\",\"authors\":\"Xiaojun Cai, Xiangyi Dai, Zhoupeng Li, Junying Chen, Xianqin Wang, Meiling Zhang\",\"doi\":\"10.1556/1326.2022.01061\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"\\n A simple, rapid, and sensitive method based on UPLC-MS/MS was developed to determine spiraeoside in mouse blood, and was applied to the pharmacokinetics and bioavailability of spiraeoside after mice after intravenous (a dose of 5 mg kg−1) and oral (a dose of 20 mg kg−1) administration. On HSS T3 column set at 40 °C, chromatographic separation was obtained with the mobile phase of acetonitrile and 0.1% formic acid using the gradient elution. Spiraeoside and internal standard (IS) were quantitatively analyzed using multiple reaction monitoring (MRM) mode in electrospray (ESI) positive interface. The MRM mode was monitoring the fragmentation of m/z 465.4→303.1 and m/z 451.3→ 289.2 for spironoside and IS, respectively. The results showed a good linear relationship was in the concentration range of 1–200 ng mL−1 (r > 0.998) and the lower limit of quantification (LLOQ) was 1.0 ng mL−1. The intra- and the inter-day precision (RSD%) of the method was within 14.0%, and the accuracy ranged from 90.0% to 115.0%. The extraction recovery of spriaeoside was better than 63.0%, and the matrix effects were in the range of 86%–98%. It also showed the half-life was short, and the absolute bioavailability was 4.0% in mice. Therefore, the established UPLC-MS/MS method was suitable for the pharmacokinetic and bioavailability study of spiraeoside in mice.\",\"PeriodicalId\":7130,\"journal\":{\"name\":\"Acta Chromatographica\",\"volume\":\" \",\"pages\":\"\"},\"PeriodicalIF\":1.7000,\"publicationDate\":\"2022-08-16\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Acta Chromatographica\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://doi.org/10.1556/1326.2022.01061\",\"RegionNum\":4,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Acta Chromatographica","FirstCategoryId":"92","ListUrlMain":"https://doi.org/10.1556/1326.2022.01061","RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
引用次数: 0
摘要
建立了一种简便、快速、灵敏的UPLC-MS/MS法测定小鼠血液中的螺旋艾酰胺,并应用于小鼠静脉注射(5 mg kg−1)和口服(20 mg kg−1)给药。在HSS T3柱上,设置为40 °C,用乙腈和0.1%甲酸的流动相梯度洗脱进行色谱分离。在电喷雾(ESI)阳性界面中,采用多重反应监测(MRM)模式对Spiraeoside和内标物(IS)进行定量分析。MRM模式是监测m/z 465.4的碎片→303.1和m/z 451.3→ 螺糖苷和IS分别为289.2。结果表明,在1–200的浓度范围内具有良好的线性关系 ng mL−1(r>0.998),定量下限(LLOQ)为1.0 ng mL−1。该方法的日内和日间精密度(RSD%)在14.0%以内,准确度在90.0%-115.0%之间。雪碧苷的提取回收率优于63.0%,基质效应在86%-98%之间。它还表明半衰期短,小鼠的绝对生物利用度为4.0%。因此,所建立的UPLC-MS/MS方法适用于螺雷酰胺在小鼠体内的药代动力学和生物利用度研究。
An UPLC-MS/MS method for quantification of spiraeoside in mouse blood and its application to a pharmacokinetic and bioavailability study
A simple, rapid, and sensitive method based on UPLC-MS/MS was developed to determine spiraeoside in mouse blood, and was applied to the pharmacokinetics and bioavailability of spiraeoside after mice after intravenous (a dose of 5 mg kg−1) and oral (a dose of 20 mg kg−1) administration. On HSS T3 column set at 40 °C, chromatographic separation was obtained with the mobile phase of acetonitrile and 0.1% formic acid using the gradient elution. Spiraeoside and internal standard (IS) were quantitatively analyzed using multiple reaction monitoring (MRM) mode in electrospray (ESI) positive interface. The MRM mode was monitoring the fragmentation of m/z 465.4→303.1 and m/z 451.3→ 289.2 for spironoside and IS, respectively. The results showed a good linear relationship was in the concentration range of 1–200 ng mL−1 (r > 0.998) and the lower limit of quantification (LLOQ) was 1.0 ng mL−1. The intra- and the inter-day precision (RSD%) of the method was within 14.0%, and the accuracy ranged from 90.0% to 115.0%. The extraction recovery of spriaeoside was better than 63.0%, and the matrix effects were in the range of 86%–98%. It also showed the half-life was short, and the absolute bioavailability was 4.0% in mice. Therefore, the established UPLC-MS/MS method was suitable for the pharmacokinetic and bioavailability study of spiraeoside in mice.
期刊介绍:
Acta Chromatographica
Open Access
Acta Chromatographica publishes peer-reviewed scientific articles on every field of chromatography, including theory of chromatography; progress in synthesis and characterization of new stationary phases; chromatography of organic, inorganic and complex compounds; enantioseparation and chromatography of chiral compounds; applications of chromatography in biology, pharmacy, medicine, and food analysis; environmental applications of chromatography; analytical and physico-chemical aspects of sample preparation for chromatography; hyphenated and combined techniques; chemometrics and its applications in separation science.