相对校正因子在中药多指标测定中的应用研究进展

中药标准物质品种和质量的相对滞后,已成为中药标准制定与提高的制约因素,为解决这一问题,不断涌现出新的测定方法。重点介绍与相对校正因子相关的一测多评法、替代对照品法、内标多控法及系统内标法等多指标定量方法;阐述了相对校正因子计算方法相关内容和技术要求,并对其在中药多指标质量控制中的应用情况进行论述。     

一测多评法同时测定胡黄连提取物中多种化学成分

目的：建立HPLC一测多评法同时测定胡黄连提取物中的10个成分,验证该方法在胡黄连质量分析中应用的科学性及可行性。方法：采用Sepax HP-C₁₈（250 mm×4.6 mm,5 μm）,流动相为乙腈-0.5%乙酸水溶液,梯度洗脱,流速1.0 mL·min ^-1,检测波长294 nm,柱温30℃。以胡黄连苷Ⅱ为内参物,建立该成分与云杉苷、草夹竹桃苷、胡黄连苷Ⅰ、胡黄连苷Ⅲ、胡黄连苷Ⅳ、黄金树苷、米内苷、6-阿魏酸梓醇、藏黄连苷B的相对校正因子,采用相对校正因子计算各成分的质量分数,同时用外标法进行测定。比较2种测定结果,评价一测多评法在胡黄连中应用的准确性及科学性。结果：10个成分在测定范围内线性良好,平均回收率在98.0%~102.0%,相对校正因子耐用性良好;采用外标法和一测多评法测定3批胡黄连提取物中10个成分含量,2种测定方法结果无明显差别。结论：以胡黄连苷Ⅱ为内标同时测定其多种成分的一测多评法可用于定量分析。     

一测多评法测定熊胆粉中多种结合型胆酸的含量

目的：建立熊胆粉中3种胆酸类成分牛磺熊去氧胆酸（TUDCA）、牛磺鹅去氧胆酸（TCDCA）和牛磺胆酸（TCA）的一测多评法,验证该方法在熊胆粉质量评价中的准确性和可行性。方法以牛磺熊去氧胆酸为内参物,确定其他两种成分相对于牛磺熊去氧胆酸的相对校正因子（Relative correction factor,RCF）,计算熊胆粉中牛磺鹅去氧胆酸和牛磺胆酸的量,实现一测多评;同时采用外标法测定熊胆粉中3种结合型胆酸的含量,比较计算值与实测值的差异。结果各相对校正因子重复性良好,一测多评法与外标法测定结果无显著差异。结论本文建立的一测多评方法操作简单,测定结果准确,可用于熊胆粉中结合型胆酸成分的定量分析。     

一测多评法测定川白芷药材中 3种香豆素成分的含量

通过建立川白芷中欧前胡素、异欧前胡素、氧化前胡素的"一测多评"含量测定方法,实验只用一个对照品同步测定川白芷中的3个成分。以欧前胡素对照品为内标物,在线性范围内,采用HPLC-DAD建立其与异欧前胡素、氧化前胡素的相对校正因子,并用该校正因子进行异欧前胡素、氧化前胡素的含量计算,实现"一测多评";同时采用外标法测定药材中这3种香豆素的含量,并比较计算值与实测值的差异。结果 20批药材中3种香豆素含量的计算值与实测值无显著差异(RSD<5%)。研究结果表明"一测多评"法控制川白芷药材的质量是可行、准确的。     

Comparative histological evaluation of two PRF formulations (PRF High and PRF Medium) on quality of life and healing outcome of apicomarginal defects: A randomized clinical trial

The objective of this randomized clinical trial was to investigate the effects of two PRF formulations (PRF High and PRF Medium) on quality of life and healing outcome (2D and 3D) of apicomarginal defects.Patients presenting with endodontic lesions and concomitant periodontal communication were randomly allocated to PRF High and PRF Medium groups. The treatment protocol in each group included a periapical surgical procedure with placement of PRF clot and membrane in the bony defect and on the denuded root surface, respectively. Quality of life was assessed for 1 week after surgery following a modified version of the patient's perception questionnaire. Postoperative pain was assessed using a visual analog scale. Clinical and radiographic evaluations were performed using Rud and Molven 2D criteria and Modified PENN 3D criteria. Buccal bone formation was assessed using sagittal and corresponding axial sections in CBCT. Histological analysis was performed using hematoxylin and eosin (H and E) staining and attaching primary antibodies to tissue sections.In total, 40 patients were enrolled in the trial (N = 20 per group). PRF Medium group patients reported significantly less swelling on the 1st (p = 0.036), 2nd (p = 0.034), and 3rd (p = 0.023) days, and average pain on the 2nd (p = 0.031), 3rd (p = 0.03), and 4th (p = 0.04) days postoperatively. The difference in success rate for periapical healing was non-significant between the PRF Medium group (89.5%) and PRF High group (90%), in both 2D and 3D imaging (p = 0.957). The formation of buccal bone was observed in five cases (26.3%) and four cases (20%) in the PRF Medium and PRF High groups, respectively, with a non-significant difference (p = 0.575). PRF Medium clots had a loose fibrin structure with a significantly higher number of neutrophils (473.79 ± 82.89 per mm²) than PRF High clots, which had a dense structure and fewer neutrophils (253.15 ± 63.86 per mm²) (p = 0.001). Autologous platelet concentrates (APCs) promoted satisfactory periapical healing, with no significant difference between the groups.Within the limitations of the study, it seems that PRF Medium should be preferred over PRF High when the patients’ quality of life is the priority.     

不同色谱条件对QAMS相对校正因子及相对保留值影响的实验研究

目的:考察不同色谱条件对"一测多评"(QAMS)相对校正因子及相对保留值的影响。方法:采用十八烷基硅烷键合硅胶色谱柱,流动相为甲醇-0.4%磷酸溶液(85∶15),检测波长254 nm,柱温30℃,流速1 mL·min-1。以大黄中5种蒽醌类成分为研究对象,测定不同色谱条件下芦荟大黄素、大黄酸、大黄酚和大黄素甲醚与内参物大黄素间的RCF和RTR。结果:5种大黄蒽醌间的RCF无显著性差异。结论:QAMS建立的蒽醌类成分间的RCF可作为一个常数用于中药或中成药中蒽醌类成分的含量测定。     

Influence of intense sound stimuli on skin microcirculation

Sound influences not only the organ of hearing but also other systems including the circulation. The purpose of the present study was to investigate the effect of strong sound on the skin microcirculation of the palmar area of the hand and of the plantar area of the foot, which are areas of dense microvasculature and rich sympathetic innervation. The laser Doppler technique was used for measuring cutaneous red cell flux (RCF). Eighteen normal subjects were studied. The results indicate that a pure tone sound of 1500 Hz, with an intensity of 100 dBA and duration 5 s, applied by earphones caused a significant decrease in RCF in 14 out of 18 subjects in the finger but not in the foot skin. A higher intensity (110 dBA) tone caused a stronger decrease of RCF in the finger. The latency and the duration of the reaction showed a dependence on the intensity of the sound, i.e. the reaction to the stronger stimulus was of shorter latency (p < 0.01) and longer duration (p < 0.05). The duration of the reaction did not show significant change when a longer stimulus of 30 s was applied. Repetitive stimuli evoked habituation (p < 0.05).     

一测多评法测定三黄片中的大黄蒽醌类成分

目的:建立一测多评法测定三黄片中大黄蒽醌类成分含量的分析方法,并进行方法学考察。方法:以三黄片为研究对象,建立大黄酸(rhein)、大黄酚(chrysophanol)和大黄素甲醚(physcion)与内参物大黄素(emodin)间的相对校正因子。分别采用外标法和一测多评法测定三黄片中4种蒽醌类成分的含量,并将一测多评法的计算值与外标法实测值用相对误差进行评价,以验证一测多评法的合理性、可行性和可重复性。结果:三黄片中蒽醌类成分间的相对校正因子分别为f 254nm大黄酸/大黄素=1.13,f 254nm大黄酚/大黄素=1.46,f 254nm大黄素甲醚/大黄素=1.01。一测多评法的计算结果与外标法的实测值之间没有显著性差异,实验所得的相对校正因子可信。结论:一测多评法可作为一个新的质量评价模式用于三黄片中蒽醌类成分的质量评价。     

“一测多评”法测定咳喘宁片中5种生物碱类成分的含量

目的建立咳喘宁片中5种生物碱类成分的一测多评含量测定方法。方法采用高效液相色谱法,色谱柱:Agilent XDB-C1(84.6 mm×150 mm,5μm),流动相为乙腈与0.1%磷酸溶液梯度洗脱,检测波长为210 nm(吗啡、磷酸可待因、盐酸麻黄碱和盐酸伪麻黄碱)与251 nm(盐酸罂粟碱),以吗啡为对照,建立吗啡与磷酸可待因、盐酸罂粟碱、盐酸麻黄碱、盐酸伪麻黄碱的校正因子,并利用该校正因子计算磷酸可待因、盐酸罂粟碱、盐酸麻黄碱、盐酸伪麻黄碱的含量,实现一测多评,同时利用外标法测定这4种成分的含量,比较两者的差异,验证一测多评法的准确性和科学性。结果采用校正因子计算的含量值与外标法实测值之间没有明显差异。结论用一测多评法对咳喘宁片进行质量控制是可行的、准确的。