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UPLC-MS/MS法测定人血浆中20（S）-原人参二醇的浓度
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| 篇名： | UPLC-MS/MS法测定人血浆中20（S）-原人参二醇的浓度 |
| TITLE： | Determination of 20（S）-protopanaxadiol Concentration in Human Plasma by UPLC-MS/MS |
| 摘要： | 目的：建立测定人血浆中20（S）-原人参二醇（简称为“PPD”）浓度的方法。方法：血浆样品经乙腈沉淀蛋白后，以非那雄胺为内标，采用超高效液相色谱-串联质谱法测定。色谱柱为WatersACQUITYUPLCHSST3，流动相为5mmol/L碳酸氢铵溶液-乙腈（梯度洗脱），流速为0.4mL/min，柱温为40℃，进样量为10μL；离子源为电喷雾离子源，以多反应监测模式（MRM）进行负离子扫描，用于定量分析的离子对分别为m/z459.40→375.20（PPD）、m/z371.30→315.30（内标）。同时将该法用于临床样品的测定。结果：PPD检测质量浓度的线性范围为0.25～30.00ng/mL（r＝0.9992），定量下限为0.25ng/mL；批内、批间RSD均小于10％，相对误差（RE）为－14.61％～12.69％；提取方法和基质效应均不影响PPD的定量测定。人参皂苷CK片100mg组、人参皂苷CK片200mg组、人参皂苷CK片300mg组类风湿性关节炎患者口服相应药物第84天时的平均cmax分别为18.06、30.03、27.00ng/mL，中位tmax分别为12.0、6.0、12.0h，平均AUC0-t分别为622.52、668.15、1155.97ng·h/mL。结论：本研究成功建立了测定人血浆中PPD浓度的方法，且方法灵敏、准确、稳定，操作简便，血浆用量少，可用于临床样本的定量测定。 |
| ABSTRACT： | OBJECTIVE ：To est ablish the method for the determination of 20（S）-protopanaxadiol（PPD）concentration in human plasma. METHODS ：Plasma samples were precipitated with acetonitrile and determined by UPLC-MS/MS ，using finandrogen as internal standard. The determination was performed on Waters ACQUITY UPLC HSS T 3 column with mobile phase consisted of 5 mmol/L ammonium bicarbonate aqueous solution-acetonitrile （gradient elution ）at the flow rate of 0.4 mL/min. The column temperature was set at 40 ℃，and sample size was 10 μL. The ion source was electrospray ion source，and negative ion scanning was carried out with multiple reaction monitoring mode . The ion pairs used for quantitative analysis were m/z 459.40→ 375.20（PPD）and m/z 371.30→315.30（internal standard ）. At the same time ，the method was applied to the determination of clinical samples. RESULTS ：The linear range of PPD was 0.25-30.00 ng/mL（r＝0.999 2），and the limit of quantitation was 0.25 ng/mL. RSDs of intra-batch and inter-batch were all lower than 10％，and relative errors （RE）were －14.61％-12.69％. Extraction method and matrix effect did not affect the quantitative determination of PPD. In ginsenoside CK 100 mg group ，ginsenoside CK 200 mg group and ginsenoside CK 300 mg group ，mean cmax of patients with rheumatoid arthritis after oral administration of corresponding drugs were 18.06，30.03，27.00 ng/mL；median tmax were 12.0，6.0，12.0 h；mean AUC 0-t were 622.52，668.15， 1 155.97 ng·h/mL. CONCLUTIONS ：The method for the determination of PPD concentration in human plasma is successfully established. The method is sensitive ，accurate， kq1907011） stable，easy to operate and less plasma consumption. It can be used for the quantitative determination of clinical samples. |
| 期刊： | 2021年第32卷第18期 |
| 作者： | 刘胜兰，唐智，陈磊，吴素芬，周玲，廖音娟，张杰 |
| AUTHORS： | LIU Shenglan ，TANG Zhi，CHEN Lei，WU Sufen，ZHOU Ling，LIAO Yinjuan ，ZHANG Jie |
| 关键字： | 20（S）-原人参二醇；超高效液相色谱-串联质谱法；蛋白沉淀法；血药浓度 |
| KEYWORDS： | 20（S）-protopanaxadiol；UPLC-MS/MS；Protein |
| 阅读数： | 172 次 |
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