HPLC测定胆石消口服液中大黄酸的含量

目的 建立测定胆石消口服液中大黄酸含量的方法.方法 采用HPLC法,色谱柱为Shim-pack-CLC-ODS(150mm ×6.0 mm,5μm),流动相为甲醇-0.1%磷酸溶液(80:20),流速1.0 ml·min-1,检测波长254 nm.结果 大黄酸的线性范围为0.006～0.500 μg(r=0.9999),平均回收率为97.09%,RSD=1.48%(n=9).结论 方法简便、分离度好、结果准确可靠,可用于胆石消口服液的质量控制.     

Rhein attenuates renal inflammatory injury of uric acid nephropathy via lincRNA-Cox2/miR-150-5p/STAT1 axis

Rhein has protective effect on uric acid nephropathy (UAN). This article aims to demystify the mechanism of function of rhein in UAN. Mouse kidney epithelial cell line (TCMK-1) was incubated with uric acid (UA) to induce inflammatory injury. Then, the TCMK-1 cells were treated with rhein. The relationships among lincRNA-Cox2, miR-150-5p and STAT1 were evaluated by luciferase reporter assay. CCK8 and flow cytometry were performed to detect cell proliferation and apoptosis. The levels of IL-6, IL-1β and TNF-α were investigated by enzyme linked immunosorbent assay. Western blot and quantitative real-time PCR were performed to examine the expression of genes and proteins. We found that UA suppressed proliferation and enhanced apoptosis and the levels of IL-6, IL-1β and TNF-α of TCMK-1 cells, which was effectively improved by rhein treatment. Furthermore, lincRNA-Cox2 overexpression caused an increase of apoptosis and inflammatory factors in the rhein-treated TCMK-1 cells. LincRNA-Cox2 regulated STAT1 expression by sponging miR-150-5p. And lincRNA-Cox2 promoted apoptosis and inflammatory injury of TCMK-1 cells by regulating miR-150-5p/STAT1 axis. In summary, our studies demonstrate that rhein has a protective effect against UAN by inhibiting renal inflammatory injury via lincRNA-Cox2/miR-150-5p/STAT1 axis.     

大黄酸及其酯化衍生物在大鼠体内的药代动力学研究

目的：研究大黄酸羧基酯化对其在大鼠体内药动行为的影响。方法：采用大黄酸甲酯和大黄酸乙酯作为模型药, 大黄酸作为阳性对照, 对大鼠单次灌胃70 mg·kg-1或者单次静注 0.7 mg·kg-1, HPLC 荧光同时监测大鼠血浆中三种分析物的血浓经时变化。结果：大黄酸甲酯和大黄酸乙酯灌胃和静注给予大鼠后, 血浆中均测不到酯类原型, 但能测到一定量的大黄酸。将甲酯和乙酯衍生物灌胃后在大鼠血浆中所测得的大黄酸成分的经时变化与直接灌胃大黄酸后大鼠血浆中大黄酸成分的经时过程相比较, 其主要的药动参数分别为：cmax （0.058 ± 0.035）、（0.95 ± 0.090）、（42.66 ± 14.41） mg·L-1 Tmax （6.7 ± 2.3）、（10.7 ± 2.3）、（0.9 ± 0.1） h t1/2β （6.0 ± 1.7）、（6.4 ± 1.0）、（3.2 ± 0.6） h AUC0-∞ （1.03 ± 0.76）、（12.79 ± 0.96）、（80.28 ± 13.59） h·mg·L-1。结论：羧基酯化降低了大黄酸在大鼠体内的有效暴露剂量, 提示此类衍生物不适于作为大黄酸的前体药物进行开发。     

大黄酸金属配合物的结构及对人肝癌HepG2细胞增殖的抑制作用

目的:以大黄酸和相应金属盐为原料,合成3种金属配合物,并对其结构进行表征,比较其抗癌活性大小。方法:采用核磁共振氢谱法、红外光谱法、紫外光谱法、滴定法、原子吸收光谱法进行结构表征;采用MTT法测试三种配合物对于人肝癌Hep G2细胞的抑制作用。结果:通过光谱法证实有配合物生成,并推测出其可能结构。MTT测试显示配合物和配体均具有一定的抗癌活性,其中大黄酸-Fe(Ⅲ)抗癌活性最强,其IC50值达17.44μg.m L-1,优于配体大黄酸(IC50=116.741μg.m L-1),大黄酸-Cu(Ⅱ)(IC50=54.427μg.m L-1),大黄酸-Cr(Ⅲ)(IC50=63.584μg.m L-1)。结论:大黄酸金属配合物抗癌活性相比配体增强。     

肾康注射液的配伍稳定性考察

摘 要 目的：考察肾康注射液与10%葡萄糖注射液的配伍稳定性。方法: 将肾康注射液与10%葡萄糖注射液的配伍液置于室温、光照（4 500Lx）和40℃恒温条件,考察不同条件下0,1,2,4,8,12,24,48 h配伍液的性状、pH、不溶性微粒,以及大黄酸和大黄素的含量。结果: 配伍液在放置过程中性状、pH无明显变化。室温条件下,配伍液在4 h后微粒数有所增加;光照和40℃恒温条件下,2 h时配伍液的微粒数明显增加。大黄酸和大黄素的含量随放置时间的延长而下降,其中大黄酸在光照条件下降最明显,大黄素在光照和40℃恒温条件下降低将近10%。结论:肾康注射液与10%葡萄糖注射液配伍后最好在4 h内输注完,滴注过程应在室温条件（10～30℃）下进行,并避免强光照射。     

RP-HPLC法测定三黄散瘀巴布剂中5种蒽醌类成分的含量

目的:建立三黄散瘀巴布剂中芦荟大黄素,大黄酸,大黄素,大黄酚,大黄素甲醚的RP-HPLC含量测定方法。方法:反相高效液相色谱法。色谱柱:Agilent Zorbax Eclipse XDB-C18(4.6 mm×150 mm,5μm);柱温25℃;流动相:甲醇-0.1%磷酸;流速:1.0 mL·min-1;检测波长:254 nm;进样量:10μL。结果:芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚分别在21.45²14.5 ng、15.68214.5 ng、15.68¹56.8 ng、18.77156.8 ng、18.77¹87.7 ng、37.40187.7 ng、37.40³74.0ng、11.05374.0ng、11.05⁸8.42 ng范围内呈良好的线性关系,平均加样回收率分别为99.82%(RSD 2.6%)、100.5%(RSD1.1%)、101.3%(RSD 1.5%)、101.5%(RSD 2.4%)、97.07%(RSD 0.80%)结论:本法稳定、可靠、操作简便、快速、重现性好,可用于三黄散瘀巴布剂的质量控制。     

HPLC法同时测定利胆排毒口服液中大黄酸、大黄素、大黄酚的含量

目的:建立HPLC法同时测定利胆排毒口服液中大黄酸、大黄素、大黄酚含量的方法.方法:采用Atlantis T3柱(150 mm×4.6 mm,3 μm),甲醇-0.05%磷酸溶液(85:15)为流动相,流速:0.8 ml·min-1,检测波长:254 nm,柱温:30℃.结果:大黄酸、大黄素、大黄酚分离度好,可排除其他物质的干扰.大黄酸在16.71～334.20 μg·ml-1的范围内有良好的线性关系,平均回收率为98.85%,RSD为0.47%;大黄素在2.06～41.28 μg·ml-1范围内有良好线性关系,平均回收率为96.95%,RSD为1.03%;大黄酚在4.46～111.60 μg·ml-1范围内有良好线性关系,平均回收率为97.97%,RSD为0.67%.结论:本方法可同时测定大黄酸、大黄素、大黄酚的含量,准确度高,重复性好,可为利胆排毒口服液质量控制提供依据.     

Antioxidant and Scavenging Activity of Emodin,Aloe-Emodin,and Rhein on Free-Radical and Reactive Oxygen Species

The objective of this study was to investigate the ability of emodin (1), aloe-emodin (2), and rhein (3) to inhibit free-radical or reactive oxygen species (.OH, ¹O₂, H₂O₂) generated in cell-free systems using isoluminol and luminol-enhanced chemiluminescence and electronic absorption spectra. In the presence of 1, 2, and 3, a dose-dependent inhibition period was observed in this system as assayed by isoluminol-enhanced chemiluminescence (ILCL) with horseradish peroxidase (HRP), as well as by luminol-enhanced chemiluminescence (LCL) with H₂O₂ or ferrous iron. On the other hand, these hydroxyanthraquinones showed an efficient scavenging activity of galvanoxyl radical in ethanolic solutions. In a separate experiment, we observed the trapping of singlet oxygen (¹O₂) generated by rose bengal in the presence of 1, 2, or 3. These results suggest that emodin, aloe-emodin, and rhein scavenge reactive oxygen and free-radical species in the following decreasing order: emodin > rhein > aloe-emodin.     

不同炮制方法对大黄中5种蒽醌类化合物含量的影响

目的：观察不同炮制方法对大黄中5种蒽醌类成分的影响,建立大黄炮制品的质量控制方法.方法：采用色谱柱为Shimadzu C18色谱柱（4.6 mm×250 mm,5 μm）,流动相为乙腈-0.1%磷酸,梯度洗脱进行测定.结果：大黄酸,大黄素、大黄粉,芦荟大黄素,大黄素甲醚加样回收率分别为98.9%（RSD=1.61%）,97.5%（RSD=1.12%）,100.6%（RSD=1.08%）,102.3%（RSD=1.78%）,101.2%（RSD=2.11%）.结论：本方法操作简单、准确,重现性好,适用于大黄饮片内在质量的评价和控制.     

HPLC法测定八正合剂中芦荟大黄素、大黄酸、大黄素和大黄酚

目的:建立高效液相色谱法同时测定八正合剂中芦荟大黄素、大黄酸、大黄素和大黄酚的含量。方法:采用Lu-na-C18(150 mm×4.6 mm,5μm);流动相:甲醇-0.1%磷酸(80:20);流速:0.8 ml/min;检测波长:254 nm;柱温:35℃。结果:芦荟大黄素、大黄酸、大黄素和大黄酚的线性范围分别为0.032μg~0.324μg、0.039μg~0.387μg、0.0104μg~0.104μg和0.0103μg~0.103μg,相关系数均为0.9999;平均加样回收率分别为98.3%、98.7%、97.7%和97.2%;RSD分别为0.9%、0.8%、1.0%和1.1%(n=6)。结论:本法专属性好,准确度、重现性好,可作为制剂的定量分析方法。