首页> 外文期刊>Journal of Chromatographic Science >Rapid Identification and Simultaneous Quantification of Multiple Constituents in Nao-Shuan-Tong Capsule by Ultra-Fast Liquid Chromatography/Diode-Array Detector/Quadrupole Time-of-Flight Tandem Mass Spectrometry
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Rapid Identification and Simultaneous Quantification of Multiple Constituents in Nao-Shuan-Tong Capsule by Ultra-Fast Liquid Chromatography/Diode-Array Detector/Quadrupole Time-of-Flight Tandem Mass Spectrometry

机译:超快速液相色谱/二极管阵列检测器/四极杆飞行时间串联质谱法快速鉴定和同时定量定量宣宣通胶囊中多种成分的含量

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摘要

A rapid and high-sensitive ultra-fast liquid chromatography coupled with a diode-array detector and a quadrupole/time-of-flight mass spectrometry (MS) method was established and validated for the chemical profiling of Nao-shuan-tong capsule (NSTC) and simultaneous quantification of five major constituents. A total of 59 components including monoterpene glycosides, flavonoids, sesquiterpenoids, ketosteroids, thiophenes, organic acids and alkaloids were identified or tentatively characterized in NSTC based on the accurate mass and tandem MS behavior. Five major bioactive constituents were chosen as the chemical indexes of holistic quality evaluation and quantified simultaneously. All calibration curves showed good linear regression (r(2) > 0.9991) in the range 25.2-510, 145-2,900, 1.84-36.8, 2.61-52.2 and 3.25-26.2 mu g/mL for gastrodin, paeoniflorin, typhaneoside, beta-ecdysterone and isorhamnetin-3- O-neohesperidoside, respectively. It also showed good precision, stability and accuracy for quantification of these five compounds. The limit of detections and limit of quantitations for the analytes ranged from 0.14 to 1.09 mu g/mL and from 0.47 to 3.63 mu g/mL, respectively. The validated quantification method was applied to analyze 10 batches of commercial NSTC. These results will provide a basis for quality control of the production process and the further pharmacological study in vivo of NSTC.
机译:建立了快速,高灵敏度的超快液相色谱,并结合了二极管阵列检测器和四极杆/飞行时间质谱(MS)方法,并验证了其对脑栓通胶囊(NSTC)的化学分析性能),并同时量化五种主要成分。根据准确的质量和串联MS行为,在NSTC中鉴定出或初步鉴定了59种成分,包括单萜糖苷,类黄酮,倍半萜类化合物,酮类固醇,噻吩,有机酸和生物碱。选择了五种主要生物活性成分作为整体质量评价的化学指标,并同时进行了定量。对于天麻素,pa药苷,鼠李糖苷,β-甜菜碱,所有校准曲线均显示良好的线性回归(r(2)> 0.9991)在25.2-510、145-2900、1.84-36.8、2.61-52.2和3.25-26.2μg / mL范围内。蜕皮甾酮和异鼠李素-3-O-新蛇皮苷。对于这五种化合物的定量也显示出良好的精密度,稳定性和准确性。分析物的检出限和定量限分别为0.14至1.09μg / mL和0.47至3.63μg / mL。验证的定量方法用于分析10批次的商业NSTC。这些结果将为NSTC的生产过程质量控制和进一步的体内药理研究提供基础。

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