白芍水提过程中芍药苷含量的NIRS快速测定研究

目的:基于近红外光谱(NIRS)技术的,建立白芍提取过程的快速质量控制方法。方法:针对白芍提取过程,以HPLC测定提取液样品中芍药苷含量,同时采集其NIRS,采用偏最小二乘(PLS)回归法建立NIRS与HPLC分析值之间多元校正模型。结果:校正模型的内部交叉验证决定系数R2为99.86,内部交叉验证均方差RMSECV为0.023 9。对提取过程中的白芍样本进行预测,结果令人满意。结论:NIRS可准确预测白芍提取过程中芍药苷含量,可推广运用于中药提取过程的快速、实时质量监控。     

HPLC法研究川芎-白芍单煎及共煎液中有效成分含量的变化

目的研究川芎-白芍单煎及共煎液中有效成分阿魏酸和芍药苷含量的变化,初步探索两味中药配伍应用的变化规律。方法采用Phenomenex Gemini C18色谱柱,以乙腈-0.2%的磷酸水溶液为流动相(梯度洗脱);流速:0.8 mL/min;柱温:35℃;检测波长分别为324 nm、233 nm,测定追踪川芎-白芍共煎液与单煎液中主要有效成分阿魏酸和芍药苷含量的变化。结果阿魏酸回归方程为Y=51.989X-11.444(r=0.9998),在11.7～210.6μg/mL范围内线性关系良好,平均加样回收率为99.58%,RSD为0.22%;芍药苷回归方程为Y=15.201X-29.802(r=0.9999),在16.1～966μg/mL范围内线性关系良好,平均加样回收率为98.67%,RSD为0.97%;川芎-白芍共煎液中阿魏酸含量比川芎单煎液中平均升高24.04%,芍药苷含量比白芍单煎液中平均升高17.47%。结论川芎-白芍共煎液中阿魏酸和芍药苷的含量高于各单煎液中含量,两者配伍具有一定的合理性。     

高效液相色谱法测定胃灵胶囊中芍药苷含量

目的建立测定胃灵胶囊中芍药苷含量的高效液相色谱法。方法采用Hypersil ODS色谱柱(150 mm×4.6 mm,10μm),流动相为乙腈-0.1%磷酸溶液(15∶85),检测波长为229 nm,流速1 mL/min,柱温30℃。结果芍药苷质量浓度在5.1～25.5μg/mL范围内与峰面积线性关系良好,r=0.999 9(n=5);平均回收率为97.30%,RSD=3.02%(n=9)。结论高效液相色谱法重现性好、简便易行,可用于胃灵胶囊的质量控制。     

高效液相色谱法测定脑心通胶囊中芍药苷的含量

目的:建立HPLC法测定脑心通胶囊的芍药苷含量测定方法。方法:采用HPLC法对脑心通胶囊中的芍药苷进行含量测定,流动相为甲醇-水(30∶70);检测波长为230nm。结果:芍药苷线性范围为104.8-524.0μg(r=0.9991,n=5),平均回收率为101.5%,RSD=1.74%。结论:该方法准确、重现性好,可用于脑心通胶囊的质量控制。     

高效液相色谱法同时测定解郁和肝胶囊中栀子苷和芍药苷的含量

目的:建立解郁和肝胶囊中栀子苷和芍药苷的HPLC含量测定方法。方法:用Diamonsil-C18色谱柱(250 mm×4.6 mm,5μm);以乙腈-0.1%磷酸溶液(14∶86)为流动相;检测波长为238 nm;柱温为25℃;流速为1.0 mL·min-1。结果:栀子苷进样量在0.16～2.42μg范围内,进样量与峰面积呈良好的线性关系,r=0.999 7,平均回收率为99.25%(n=6);芍药苷进样量在0.12～1.82μg范围内,进样量与峰面积呈良好的线性关系,r=0.999 5,平均回收率为98.87%(n=6)。结论:本方法操作简便,结果准确,重现性好,可作为该制剂的含量测定方法。     

HPLC法测定丹栀逍遥片中芍药苷的含量

目的建立丹栀逍遥片中芍药苷的含量测定方法。方法采用高效液相色谱法。色谱柱:Kromasil C18柱(200mm×4.6mm,5μm);流动相:甲醇-水(用磷酸调节pH值至3.5)(13∶87);流速:1.0mL.min-1;柱温:室温;检测波长:230nm。结果芍药苷在0.28～1.76μg范围内线性关系良好,相关系数r=0.998 5,平均加样回收率为98.6%(RSD=2.2%)。结论该方法快速简便,结果准确,可用于其质量控制。     

不同贮藏年限白芍的化学成分分析

目的比较不同贮藏年限白芍的化合物含量变化。方法采用HPLC法,测定不同贮藏年限的白芍中芍药苷、芍药苷亚硫酸酯、芍药内酯苷和没食子酸的含量。结果芍药苷、芍药苷亚硫酸酯的含量变化与贮藏时间长短无明显相关性,芍药内酯苷含量随贮藏时间的延长存在降低的趋势,没食子酸含量变化不明显。结论白芍可贮藏的年限较长,但采用硫磺熏蒸会大大降低芍药苷的含量。     

Paeoniflorin inhibits the histaminergic system and promotes non-rapid eye movement sleep via adenosine A1 receptors

Insomnia is a common disorder seen in nearly 30%-35% of the general population worldwide,with a range of 10%-15% being assessed as moderate to severe disorders.Symptoms of insomnia include poor sleep quality,difficulty in falling asleep,frequent awakenings during the night and early morning awakenings.Insomnia give rise to fatigue,irritability,impaired concentration and reduced alertness,causing serious impact on the quality of life of affected individuals.Current pharmacological treatment of insomnia involves the use of sedative-hypnotic benzodiazepines(BZ) and non-benzodiazepine drugs(Z-drugs).Z-drugs are the first line of management followed by BZ,amitryptiline and antihistamines.Insomnia could be effectively treated by the Z-drugs,such as zolpidem and the BZ,but their multiple adverse effects hamper their application.Paeoniflorin {PF,5beta-[(Benzoyloxy)methyl]tetrahydro-5-hydroxy-2-methyl-2,5-methano-1H-3,4-dioxacyclobutapentalen-1alpha(2H)-yl-beta-D-glucopyranoside,C23H28O11} is one of the principal active ingredients of Paeonia Radix.PF possesses inhibitory effects in the nervous system,such as suppress spike discharges and analgesic effect.These observations indicate that PF might have a potent sleep promoting effect.The aim of this study was to determine whether PF could modulate sleep behaviors by recording EEG and electromyogram in mice.The results showed that PF 25 and 50 mg·kg-1 could significantly shorten the sleep latency;increase the amount of non-rapid eye movement(non-REM,NREM) for 3 h,with an increase in the number of NREM and REM sleep episodes.PF 25 and 50 mg·kg-1 increased the number of bouts of wakefulness but decreased their duration.On the other hand,PF increased the number of state transitions from wakefulness to NREM sleep and subsequently from NREM sleep to wakefulness.However,PF had no effect on the amount of REM sleep.Immunohistochemical study showed that PF increased c-Fos expression in the neurons of ventrolateral preoptic area(VLPO),a sleep center in the anterior hypothalamus,and decreased c-Fos expression in the arousal tuberomammillary nucleus(TMN),which was located in the caudolateral hypothalamus.The sleep-promoting effects and changes in c-fos induced by PF were reversed by CPT,an antagonist at the adenosine A1R.We found a high degree of colocalization between histaminergic and gabaergic neurons in GAD 67-GFP mice TMN.Then we use GAD 67-GFP mice to help indentify histaminergic neurons.PF inhibited histaminergic neurons in the TMN by whole-cell patch clamping in the brain slice,CPT totally blocked the histaminergic neurons inactivation induced by PF.These results indicate that PF increased NREM and REM sleep by inhibiting the histaminergic system via A1R,suggesting its potential application for the treatment of insomnia.     

高效液相色谱法测定复光颗粒中芍药苷含量

目的 建立复光颗粒中芍药苷的含量测定方法.方法 采用高效液相色谱法,流动相为甲醇-0.05 mol/L磷酸二氢钾溶液(35:65),检测波长为230 nm,柱温为30℃.结果 芍药苷质量浓度线性范围为0.075～40 g/L,平均回收率为98.66%,RSD＝0.62%(n＝6).结论 该方法可靠、简单可行,为控制复光颗粒的内在质量提供了科学依据.     

基于5组分测定和6波长高效液相色谱指纹谱的双标定量指纹法建立六味地黄丸对照指纹图谱动态技术标准研究

目的 建立双标定量指纹法精确恢复对照指纹图谱(RFP)理论和方法,实现动态指纹图谱标准的校正和复原.方法 用RP-HPLC法对LWDHW中5组分进行定量分析和建立其6波长定量指纹图谱研究.结果 利用HPLC-DAD在最大吸收波长处同时测定了没食子酸、5-羟甲基糠醛和丹皮酚含量,结合等吸收双波长消去法对色谱峰完全重叠的芍药苷和马钱苷进行同时定量测定,建立210、230、246、265、280和310 nm LWDHW-HPLC指纹谱,用均值法整合6波长HPLC定量指纹谱.以5组分测定和6波长指纹谱鉴定结果分别聚类分析比较不同厂家产品质量差异,结果以后者更为准确可靠,在此基础上建立LWDHW双标定量指纹法技术标准.结论 基于多指标定量分析和平行多波长高效液相色谱指纹谱的双标定量指纹法能够找到产生RFP的标准制剂和实现实时随行定量检测LWDHW指纹图谱.这一方法再现了中药指纹图谱标准,为中药指纹图谱工业化整体定量控制中药质量建立了可行技术方法,是中药指纹图谱评价方法发展历程中的一次技术飞跃.