酸枣仁中斯皮诺素、酸枣仁皂苷A含量测定及其质量等级划分标准研究

目的:建立同时测定酸枣仁中斯皮诺素、酸枣仁皂苷A含量的方法,并进行质量等级划分。方法:采用高效液相色谱-蒸发光散射检测法测定含量。色谱柱为Inertsil ODS-SP,流动相为乙腈-水(梯度洗脱),流速为1.0 m L/min,柱温为30℃,漂移管温度为90℃,载气流速为2.9 L/min,进样体积为20μL。以药材样品厚度、宽度、长度、百粒质量为指标,考察其外观性状;采用SPSS22.0软件分析样品中斯皮诺素、酸枣仁皂苷A含量及其外观性状与中药质量常数的相关性,并建立该药材的质量等级划分标准。结果:斯皮诺素、酸枣仁皂苷A的质量浓度线性范围分别为1.03~6.18μg/mL(r=0.999 7)、1.05~6.30μg/mL(r=0.999 8);定量限分别为0.171、0.174μg/mL,检测限分别为0.052、0.053μg/mL;精密度、稳定性、重复性试验的RSD均小于2%;加样回收率分别为99.01%~102.97%(RSD=1.39%,n=6)、97.94%~101.03%(RSD=1.13%,n=6)。相关性分析结果显示,药材长度、宽度、百粒质量、斯皮诺素含量、酸枣仁皂苷A含量均与其中药质量常数呈正相关。质量等级划分结果显示,30批样品中S1~S4、S7~S12为一等品;S5、S6、S13~S17、S20~S30为二等品;S18、S19为三等品。结论:所建含量测定方法操作简单,精密度、准确度、稳定性均较好,可用于同时测定酸枣仁中斯皮诺素、酸枣仁皂苷A的含量;所建酸枣仁质量等级划分标准可用于综合评价该药材质量。     

不同贮藏条件下吴茱萸饮片稳定性考察

目的 考察吴茱萸饮片的贮藏稳定性及指标性成分吴茱萸碱、吴茱萸次碱、柠檬苦素含量在不同干燥、光照、避光条件下的稳定性。方法 分别采用牛皮纸袋、真空和非真空聚乙烯塑料袋包装12批吴茱萸饮片，分别在温度为16～17℃、相对湿度为50%～60%的药品阴凉柜中贮藏0～3年，按2020年版《中国药典（一部）》标准方法测定性状、水分、浸出物，并采用高效液相色谱法测定饮片中吴茱萸碱、吴茱萸次碱、柠檬苦素分别在0,60,80,105℃干燥，159 lx照射0,4,8,16,32 h，室温避光放置0,1,3,5 d条件下的含量。结果 随着贮藏时间的延长，吴茱萸饮片的性状均无显著变化，水分为9.34%～14.13%，浸出物为42.75%～51.15%；吴茱萸碱和吴茱萸次碱的总含量为0.35%～5.02%，整体呈升高趋势；柠檬苦素含量为0.08%～1.81%，整体呈降低趋势，其中2批含量不符合标准规定（不得少于0.20%）。含量稳定性试验结果显示，吴茱萸碱、吴茱萸次碱、柠檬苦素在不同干燥及避光条件下的含量分别为0.94%～0.96%、0.56%～0.57%、0.52%～0.54%和0.96%～0.97%、0....     

清心安神桂仁茶的质量标准研究

目的研究清心安神桂仁茶的质量标准。方法 (1)采用TLC法对茶剂中的斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷B、茯苓和龙眼肉等进行鉴别;(2)采用HPLC法对茶剂中的斯皮诺素进行定量,使用Intersil C18色谱柱(250mm×4.6mm,5.0μm);以乙腈-水(12∶88)为流动相进行梯度洗脱;检测波长为335nm。结果 (1)茶剂中的斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷B、茯苓和龙眼肉的TLC鉴别专属性强;(2)斯皮诺素的线性方程、相关系数(r)与线性范围分别为y=429 563x-236 697,r=0.999 6,3.10~620.00μg·mL~(-1);平均加样回收率与RSD值分别为96.07%和1.39%;(3)3批制剂中斯皮诺素的平均含量及其RSD值分别为90.60μg·g-1和1.34%。结论所建立的清心安神桂仁茶质量标准可用于该茶剂的质量控制。     

正交试验优化酸枣仁中5种活性成分的超声离心提取工艺

目的 通过单因素和正交试验设计，对酸枣仁中5种活性成分的超声离心提取工艺进行优化。方法 选择甲醇浓度、液固比、提取时间3个因素，采用单因素和正交表L₉(3⁴)进行试验，以斯皮诺素、6’"-阿魏酰斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷B和白桦脂酸的峰面积为指标，进行综合评价。结果 酸枣仁最佳超声离心提取工艺为甲醇浓度80%、液固比7∶1(mL·g^-1)、提取时间40 min。结论 该提取工艺稳定可行，能够有效提取酸枣仁中活性成分，便于后续快速含量测定研究。     

UPLC-MS法测定酸枣仁炮制前后的12种成分

目的 测定不同来源酸枣仁在炒制前后斯皮诺素、6-阿魏酰斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷B、白桦脂酸、当药黄素、柚皮苷、异槲皮苷、芦丁、槲皮素、阿魏酸、异牡荆苷等12种成分的含量。方法 采用UPLC-MS技术，以乙腈(A)-水(B)为流动相，经Waters Acquity UPLC BEH C₁₈色谱柱(100 mm×2.1 mm, 1.7μm)梯度洗脱，流速0.3 mL·min^-1,柱温30℃,样品室温度8℃,进样量1.0μL。离子源用负离子模式进行扫描采集，用MRM模式监测。结果 12种成分在相应的进样量范围内线性关系良好，r²≥0.9990,方法精密度、重复性、稳定性的RSD值均小于2.0%,平均加样回收率为98.37%～101.34%,RSD为0.49%～2.82%。结论 所用方法快速、准确，可用于酸枣仁生品及炮制品的质量评价，为优化酸枣仁的炮制工艺提供了依据。     

不同包装工艺对薄荷挥发油稳定性的影响

目的研究不同包装工艺对薄荷挥发油稳定性的影响。方法对普通包装和真空包装的薄荷在37℃和相对湿度75%的条件下保存三个月,每月考察其挥发油含量。结果真空包装的薄荷挥发油含量较普通包装高。结论真空包装更有利于薄荷贮存质量稳定性,是一种较好的保质贮藏方式。     

不同包装工艺对薄荷挥发油稳定性的影响

目的研究不同包装工艺对薄荷挥发油稳定性的影响。方法对普通包装和真空包装的薄荷在37℃和相对湿度75%的条件下保存三个月,每月考察其挥发油含量。结果真空包装的薄荷挥发油含量较普通包装高。结论真空包装更有利于薄荷贮存质量稳定性,是一种较好的保质贮藏方式。     

他米巴罗汀原料药的稳定性考察

目的考察他米巴罗汀原料药的稳定性。方法依据2010年版《中国药典（二部）》附录“原料药与药物制剂稳定性试验指导原则”的有关技术要求,进行稳定性试验,包括影响因素试验、加速试验、长期试验。结果两年考察结果显示,3批样品的熔点、含量、有关物质均无显著变化,外观上稍有吸湿性。结论他米巴罗汀原料药应密闭于阴凉干燥处贮藏,有效期暂定两年。     

基于UPLC-Q-TOF-MS技术的酸枣仁水提物中8种有效成分的体内组织分布研究

本文旨在研究酸枣仁中8种有效成分的组织分布差异,为其药效物质基础研究提供参考。建立超高效液相色谱-四级杆-飞行时间质谱(UPLC-Q-TOF-MS)测定大鼠组织中8种有效成分的含量测定方法,并应用于正常大鼠灌胃给予酸枣仁水提物(15 g·kg^-1)后,心、肝、脾、肺、肾、肌肉、脑、小肠和血清中8种有效成分在0.5、1.0、2.0 h的组织分布特点。结果显示, 8种成分在所设浓度范围内线性关系良好(r> 0.994 6);各成分的日内、日间精密度均小于19.77%,准确度均在-19.68%～19.46%;提取回收率均在86.70%～114.29%,基质效应均在82.14%～114.57%。4种黄酮当药黄素、斯皮诺素、6?-阿魏酰斯皮诺素、山柰酚-3-O-芸香糖苷主要分布在小肠>肾>心>肝中; 3种四环三萜类酸枣仁皂苷A (JuA)、酸枣仁皂苷B (JuB)、酸枣仁皂苷A1 (JuA1)主要分布在小肠>肺>脾>肾脏中;五环三萜类皂苷白桦脂酸主要分布在小肠>心>肺>肾>肝中。酸枣仁黄酮和皂苷类成分均能以极...     

酸枣仁中掺理枣仁的高效液相色谱法鉴别方法研究

目的 建立测定酸枣仁和理枣仁中6’’’-芥子酰斯皮诺素含量的高效液相色谱法（HPLC）,以鉴别酸枣仁中掺伪理枣仁。方法 2020年12月至2022年12月,采用HPLC法,选用Agela Venusil ASB C18柱（4.6 mm×200 mm,5μm）;以乙腈-0.2%冰醋酸水溶液为流动相梯度洗脱,对酸枣仁及理枣仁中6’’’-芥子酰斯皮诺素的含量进行分析测定;检测波长：335 nm;体积流量：1.0 mL/min,柱温为30℃。结果 6’’’-芥子酰斯皮诺素在2.32～138.96μg/L(r=1)内呈良好的线性关系。理枣仁平均加样回收率为97.5%,相对标准偏差（RSD）为1.5%。酸枣仁平均加样回收率为97.8%,RSD为1.7%。6’’’-芥子酰斯皮诺素在酸枣仁中含量范围为0.003 3%～0.005 1%,在理枣仁中含量范围为0.050 6%～0.066 0%。结论 建立的6’’’-芥子酰斯皮诺素HPLC含量测定分析方法灵敏度高、专属性强、重现性好,可用于酸枣仁中掺伪理枣仁的鉴别研究。     

A novel spinosin derivative from Semen Ziziphi Spinosae

A novel spinosin derivative, 6?-(4?'-O-β-D-glucopyranosyl)-vanilloyl spinosin (1) was isolated from the methanol extract of Semen Ziziphi Spinosae, together with five known flavonoids, swertish, spinosin, 6?-feruloylspinosin, isospinosin and kaempferol 3-O-α-L-rhamnopyranosyl-(1 → 2)-O-[O-α-L-rhamnopyranosyl-(1 → 6)]-β-D-glucopyranoside, and two alkanoids, zizyphusine and 6-(2',3'-dihydroxyl-4'-hydroxymethyl-tetrahydro-furan-1'-yl)-cyclopentene[c]pyrrole-1,3-diol. The structure of compound 1 was elucidated by spectroscopic methods including UV, IR, ESI-TOF-MS, 1D, and 2D NMR techniques.     

酸枣仁皂苷提取物的制备与酸枣仁皂苷A和B的含量测定

目的优化酸枣仁总皂苷的大孔吸附树脂纯化工艺;并进一步建立RP-HPLC法同时测定酸枣仁皂苷提取物中酸枣仁皂苷A和B的含量。方法采用单因素方法对纯化工艺条件进行优化,得到酸枣仁皂苷提取物,进而建立RP-HPLC法对酸枣仁提取物中酸枣仁皂苷A和B进行含量测定。结果最佳纯化工艺为:采用AB-8型大孔吸附树脂进行纯化,上样吸附时间为1.5 h,洗脱流速为1.0 mL.min-1,体积分数为70%的乙醇溶液洗脱160 mL。采用此纯化方法得到的酸枣仁皂苷提取物中皂苷的质量分数为52%,测得其酸枣仁皂苷A和B的含量质量分数分别为2.298%和0.789%。酸枣仁皂苷提取物中酸枣仁皂苷A和B的质量浓度分别在14.7～293.0 mg.L-1(r=0.999 7,n=6)、7.2～144.0 mg.L-1(r=0.999 6,n=6)内与峰面积呈良好线性关系;平均回收率(n=9)分别为103.7%、101.9%。结论该工艺稳定可行且提取物中皂苷含量高,具有广泛的应用前景;建立的RP-HPLC法可为酸枣仁皂苷提取物质量标准的建立提供一定依据。     

热浸酸枣仁戒断治疗安眠药物依赖性成瘾42例

目的:探讨酸枣仁热浸法,戒断治疗因服用西药催眠药所致的依赖性成瘾的疗效.方法:治疗组42例用保温水瓶,热水(95℃)浸泡酸枣仁4～5 h,代"水"频服.对照组28例,口服安神补心丸及睡前服用地西泮.结果:治疗组42例因失眠服用西药出现依赖性成瘾的患者,显效30例,有效9例,无效3例.跟踪调查显效、有效患者中,未见停服西药催眠药的戒断症状.对照组仍需服地西泮.结论:使用方法简便;酸枣仁可作为治疗失眠症和西药依赖性成瘾戒断治疗的有效方药.     

酸枣仁总皂苷抗抑郁作用的实验研究

目的研究酸枣仁总皂苷对行为绝望小鼠抑郁模型的影响。方法采用小鼠强迫游泳实验和悬尾实验抑郁模型,小鼠行为绝望的不动时间作为指标,考察酸枣仁总皂苷抗抑郁活性。结果酸枣仁总皂苷中、高剂量组均能减少小鼠强迫游泳和悬尾不动时间,与空白对照组比较差异有统计学意义(P<0.05,P<0.01)。结论酸枣仁总皂苷具有一定的抗抑郁作用。     

Two new flavonoid glycosides from Semen Ziziphi Spinosae

Two novel flavonoid glycosides, 6"'-dihydrophaseoylspinosin (1) and 6″,6"'-diferuloylspinosin (2), were isolated from the MeOH extract of Semen Ziziphi Spinosae, together with six known flavonoids, isovitexin-2″-O-β-(6-O-E-feruloyl)glucopyranoside (3), spinosin (4), isospinosin (5), 6"'-feruloylspinosin (6), swertisin (7), and isovitexin-2″-O-β-d-glucopyranoside (8). The structures of 1 and 2 were elucidated by spectroscopic methods including UV, IR, ESI-TOF-MS, 1D NMR, and 2D NMR experiments.     

灰关联度法评价中药酸枣仁的质量

目的建立中药酸枣仁的质量评价方法。方法通过测定不同品种和产地酸枣仁药材中黄酮、皂苷、多糖和脂肪油的含量,采用灰关联度法,以定义的相对关联度为测度,构建质量评价模型,并与传统经验鉴别结果相比较。结果对14批样品进行质量排序,优劣情况与经验鉴别结果一致。结论本方法可用于中药酸枣仁的综合性质量评价。     

A novel spinosin derivative from Semen Ziziphi Spinosae

A novel spinosin derivative, 6?-(4?′-O-β-d-glucopyranosyl)-vanilloyl spinosin (1) was isolated from the methanol extract of Semen Ziziphi Spinosae, together with five known flavonoids, swertish (2), spinosin (3), 6?-feruloylspinosin (4), isospinosin (5) and kaempferol 3-O-α-l-rhamnopyranosyl-(1 → 2)-O-[O-α-l-rhamnopyranosyl-(1 → 6)]-β-d-glucopyranoside (6), and two alkanoids, zizyphusine (7) and 6-(2′,3′-dihydroxyl-4′-hydroxymethyl-tetrahydro-furan-1′-yl)-cyclopentene[c]pyrrole-1,3-diol (8). The structure of compound 1 was elucidated by spectroscopic methods including UV, IR, ESI-TOF-MS, 1D, and 2D NMR techniques.     

Pharmacokinetics and tissue distribution of spinosin after intravenous administration in rats

Spinosin is the major effective single constituent in the traditional Chinese herb Semen Ziziphi Spinosae, which is used for sedation and hypnosis. For the further use of spinosin in treating insomnia, the pharmacokinetics and tissue distribution of spinosin after intravenous administration to rats was investigated. An HPLC method with an ODS column (250 mm x 4.6 mm, i.d.) and a mobile phase of acetonitrile-water-acetic acid (23:77:1) was used for the determination of spinosin in the plasma and tissues of rats. Vanillin was used as an internal standard, and spinosin was detected at 334 nm. The calibration curve of spinosin in plasma showed good linearity over the concentration range of 1-300 microg/ml, and the quantitation of limit of plasma was 1 microg/ml. The linear range of concentrations of spinosin in the heart, spleen, stomach, lung, testis, brain, and intestine was 0.1-40 microg/ml and the quantitation limit was 0.1 microg/ml. The linear range of concentrations of spinosin in the liver and kidney was 1-150 microg/ml, and the quantitation limit was 1 microg/ml. The correlation coefficients of all calibration curves were between 0.9939 and 0.9980. The intra and interrun precision for all samples was less than < or =11.0%. The time-concentration curve of spinosin after the intravenous administration of a single dose of 20 mg/kg to rats corresponded to the two-compartment model. The main pharmacokinetic parameters T(0.5alpha), T(0.5beta), CLs, AUC(0-T), and V(c) were 6.66 min, 51.5 min, 1.42 l.min(-1), 2.83 mg.min.ml(-1), and 14.0 l.kg(-1), respectively. At 20 min, a concentration peak occurred in liver and brain tissues. The highest level of spinosin occurred in the liver, followed by the spleen and kidney. The lowest level of spinosin appeared in the testis, followed by the brain. Spinosin was not detected in smooth and skeletal muscle. After intravenous administration, the drug was distributed extensively and transferred quickly in rats in vivo.     

LC-MS-MS法测定4种中药中的呕吐毒素

目的：建立酸枣仁、淡豆豉、薏苡仁、补骨脂等4种中药中呕吐毒素的高效液相色谱-串联三重四极杆质谱（ LC-MS-MS）测定方法。方法：样品经水提取、免疫亲和柱净化后,用LC-MS-MS法进行分析测定。结果：呕吐毒素在2-50 ng·;ml-1范围内进样量与峰面积呈良好的线性关系,r＞0.999,加样回收率在68.7%-88.3%之间。结论：本法简便快速、灵敏度高、结果准确,可用于酸枣仁等4种中药中呕吐毒素的测定分析。     

Identification and discrimination of Ziziphi Spinosae Semen and Ziziphi Mauritianae Semen based on HPLC fingerprint analysis

A simple, reproducible and reliable HPLC fingerprint analysis method of Ziziphi Spinosae Semen (ZSS) and Ziziphi Mauritianae Semen (ZMS) was established, and then it was applied to analyze samples collected from different locations. A total of 12 common fingerprint peaks were designated in ZSS and ZMS, respectively, and five of which were definitely identified. Of these common peaks, 10 peaks were presented in both ZSS and ZMS, whereas two were characteristic for ZSS and ZMS, respectively.Furthermore, the two characteristic peaks of ZMS were definitely assigned as 6′′′-sinapoylspinosin and frangufoline by HPLC guided purification and structural elucidation. The HPLC fingerprint analysis was proved to be useful in identifying and discriminating ZSS and ZMS, which was beneficial for quality control of ZSS and its products.