四川纳溪地区栀子指纹图谱及红花苷和栀子苷含量的研究

目的 研究四川纳溪地区栀子的指纹图谱,并测定西红花苷和栀子苷的含量.方法 采用HPLC法建立了栀子的指纹图谱并测定不同结构西红花苷和栀子苷的含量.结果 各地栀子药材与对照指纹图谱的相似度分别为0.993、0.993、0.995、0.978、0.999、0.989、0.999、0.998、0.999、0.996.不同产地栀子的栀子苷含量均在2.62%以上,平均含量为3.03%.西红花总苷含量最低为1.20%,最高为2.01%,平均含量1.63%.结论 各产地栀子药材表现出较高的相似度,说明纳溪地区栀子药材所含化学成分随产地的变化小;栀子苷的含量均高于国家药典1.8%的要求,符合药用标准.西红花苷-1的含量在不同产地栀子中差异较大,但其占西红花总苷的百分比比较稳定,约为65%.     

GAP基地与普通产地栀子中栀子苷的含量比较

目的测定来源于GAP基地栀子药材与普通产地栀子药材中栀子苷的含量。方法采取HPLC法:Kroma-sil C18柱,乙腈-水(15∶85)为流动相,流速1 mL.min-1,柱温25℃,检测波长238 nm。结果GAP基地的栀子苷含量比普通产地的要高,含量波动小,稳定,且远高于药典标准。结论经GAP栽培的药材栀子苷含量稳定,实施药材GAP规范化种植值得推广。     

10批栀子中环烯醚萜苷类成分含量测定

目的 测定不同产地的10批栀子药材中栀子苷、京尼平龙胆二糖苷及总环烯醚萜苷含量。方法 采用HPLC测定栀子苷、京尼平龙胆二糖苷含量;采用紫外分光光度法测定总环烯醚萜苷含量。结果 江西产栀子中环烯醚萜苷类成分含量高。结论 不同产地栀子药材中环烯醚萜苷类成分含量有所差别。     

不同干燥方法对栀子药材中两种化学成分含量的影响

目的 评价不同干燥方法 对生药栀子中两种主要成分含量的影响.方法 采用100℃烘干、50℃烘干、冷冻干燥、蒸后烘干、减压干燥、微波干燥6种方法 处理栀子药材,采用RP-HPLC法测定栀子中两种主要成分栀子苷和西红花苷-1.结果 定量分析了6种干燥方法 炮制的栀子药材中两种主要成分的含量.结论 不同干燥方法 对栀子药材中栀子苷和西红花苷-1的含量有一定影响,50℃烘干对两类成分的保存均具有较好的效果,冷冻干燥、减压干燥、100℃烘干效果一般,蒸后烘干和微波干燥对栀子苷的保存效果较好.     

用RP-HPLC法测定不同产地独一味药材中山栀子苷甲酯的含量

目的：建立测定不同产地独一味药材中山栀子苷甲酯含量的RP-HPLC方法。方法：采用SymmetryC18色谱柱（150mm×4.6mm,5μm）,流动相：甲醇-水（25：75）,流速：1.0ml/min,检测波长：238nm。结果：山栀子苷甲酯在5.0～50μg/ml（r=0.9998）线性关系良好,加样回收率为94.7%,RSD为2.8%。9批不同产地独一味药材中山栀子苷甲酯的含量为0.12%～1.30%,甘肃玛曲县所产独一味的除根以外的部分的山栀子苷甲酯的含量最高（1.30%）。结论：本方法准确、可靠,适于独一味药材中山栀子苷甲酯含量的测定。不同产地独一味药材中山栀子苷甲酯含量存在较大差异。     

HPLC同时测定栀子中的4种成分

目的 采用HPLC法同时测定栀子类药材中绿原酸、栀子苷、西红花苷Ⅰ和西红花苷Ⅱ的含量.方法 采用Waters C18色谱柱(250mm×4.6 mm,5μm),以甲醇-0.2％磷酸溶液为流动相,梯度洗脱,流速1 mL· min-1,绿原酸、栀子苷的检测波长分别为325、238 nm,西红花苷Ⅰ和西红花苷Ⅱ的检测波长为441 nm.结果 绿原酸、栀子苷、西红花苷Ⅰ和西红花苷Ⅱ的线性范围分别为0.01 ～ 10.0、0.25～ 25.0、0.15 ～ 15.0、0.075 ～ 7.50 μg· mL-1,平均回收率分别为101.57％、101.04％、100.66％、99.58％.结论 所用方法分离效果好,操作简便,可为栀子类药材的质量控制提供方法.     

栀子药材中栀子苷的含量测定

目的　比较药材栀子中栀子苷的含量。方法　采取RP -HPLC法 ,ODS柱 ,甲醇 -水 (1∶1)为流动相 ,检测波长 340nm ,测定的不同产地、不同品种共 12批栀子的栀子苷含量。结果　浓度在 5 75～ 4 6 μg·ml- 1 范围内 ,栀子苷的峰面积与进样量呈良好的线性关系 (r=0 9997) ,平均回收率为 10 1 2 % ,RSD =1 5 3%。结论　该法简便 ,准确、重复性好 ,可作为栀子的质量控制方法     

接骨合剂的质量控制

目的:制定桃红接骨合剂的质量控制方法.方法:对处方中的三七、栀子等药材进行薄层色谱鉴别,采用高效液相色谱法测定黄芩药材中黄芩苷含量.结果:黄芩苷在0.011 96～0.191 4 mg·mL-1范围内具有良好的线性关系;平均回收率为100.43%(RSD为0.89%).结论:本制剂质量控制方法可行.     

RP-HPLC法测定蒙药五味沙棘散中栀子苷的含量

五味沙棘散是由蒙药沙棘膏、木香、白葡萄干、甘草、栀子五味药材制成的蒙药制剂。具有清热祛痰,止咳定喘之功效。用于肺热久咳,胸中满闷,胸胁作痛慢性支气管炎见上述证候者。笔者选用栀子苷作为含量指标,建立了蒙药五味沙棘散中栀子苷的含量测定方法。 1 仪器与试药     

不同产地仙茅药材薄层层析鉴别及仙茅苷的含量测定

目的:分析不同产地仙茅药材的化学成分并测定其中仙茅苷的含量。方法:以醋酸乙酯-甲醇-甲酸(10:1:0.1)为展开剂,2％三氯化铁-2％铁氰化钾(1:1)为显色剂,对各地产仙茅药材化学成分比较分析;以薄层层析-紫外分光光度法测定仙茅苷含量。结果:各地产仙茅药材均含有仙茅苷,但其它化学成分不尽相同;含量为:1.52g‰(四川宜宾)、0.65‰(云南大关)、0.42‰(湖献溆浦)、1.39‰(广东)、0.57‰(广西)、0.24‰(贵州凯里)。结论:各地产仙茅药材化学成分不尽相同;仙茅苷含量以四川宜宾产为最高。     

市售栀子饮片的质量评价研究

目的 考察市售栀子饮片的质量。方法 收集50批不同厂家生产的栀子,应用RP-HPLC波长切换法同时测定栀子苷、西红花苷Ⅰ与西红花苷Ⅱ的含量;依据《中国药典》2015年版一部品种项下规定的方法测定水分、总灰分;采用原子吸收分光光度法测定其中18批样品中镉元素的含量。结果 50批栀子中总灰分和栀子苷均符合标准规定;水分有2批不符合标准规定;西红花苷Ⅰ的含量为0.31%～1.35%、西红花苷Ⅱ的含量为0.04%～0.63%;18批栀子中镉元素有3批超出千万分之三的限度。结论 大部分栀子饮片符合药典标准,质量情况较为乐观。栀子成分复杂多样,仅以其中环烯醚萜类的栀子苷作为质控指标稍欠全面,无法很好地反应出该品种的质量优劣,建议修订完善标准。     

肝炎净注射液质量标准的研究

目的 制定肝炎净注射液的质量标准。方法 对栀子、黄芩、茵陈进行了薄层鉴别。用高效液相色谱法测定了制剂中栀子苷的含量。固定相为Shim Pack ODS C18柱，以乙腈-水(12：88)为流动相，检测波长240nm。结果 栀子苷在0．0797～3．9872μg内呈良好的线性关系。栀子苷的平均回收率为99．92％(n=5)，RSD为1．22％。结论 方法简便、准确、重现性好。可用于控制肝炎净注射液质量。     

正交设计法优选烘法炮制焦栀子的工艺

目的 优选烘法炮制焦栀子的工艺参数.方法 采用正交试验法考察炮制温度、烘制时间、堆放厚度、粉末细度等影响因素,以焦栀子的色泽、浸出物与栀子苷的含量作为评价指标,综合评分,优选其工艺条件.结果 炮制温度对实验结果有显著性影响,其最佳炮制工艺为160℃,烘10 min,堆放厚度2cm,过1号筛粉末.结论 优选出的焦栀子炮制工艺能较好地保证其炮制品的质量.     

高效液相色谱法测定江津栀子中栀子苷含量

目的建立测定江津栀子中栀子苷含量的高效液相色谱法。方法色谱柱为UltimateTM C18键合硅胶柱(250 mm×4.6 mm,5μm),流动相为乙腈-水(10∶90),流速1.0 mL/min,温度25℃,检测波长238 nm。结果栀子苷进样量在3.2～11.2μg范围内与峰面积呈良好的线性关系,回归方程为Y=-439 843.76+1 012 294.70 X,r=0.999 2(n=5);平均加样回收率为99.34%,RSD=1.49%(n=6)。结论高效液相色谱法测定江津栀子中栀子苷的含量,操作简便、结果稳定,精密度、重现性、回收率均较好。     

Simultaneous determination of bioactive marker compounds from Gardeniae fructus by high performance liquid chromatography

Gardeniae fructus is one of the medicinal herbs that have been used in Far Eastern countries, such as Korea, China, and Japan. Gardeniae fructus is the dried ripe fruit of Gardenia jasminoides Ellis (Rubiaceae) and has been used as a yellow dye. It is widely used as traditional herbal medicine for reducing fever, cholagogue, diuretic and antiphlogistic effects. We established an analytical method that was useful to evaluate the quality control, and standardize quantification monitoring of 68 samples of Gardeniae fructus collected from Korea and China. While numerous previous studies have focused on the simultaneous analysis of geniposide, which constitutes the higher proportion of Gardeniae fructus, and crocin, which determines its color, no simultaneous analysis of gardenoside and geniposide, the major components of Gardeniae Fructus, has been performed. However, previously reported methods are not considered accurate enough because only geniposide or gardenoside was chosen to be the marker component for the quality control of Gardeniae fructus. Thus, we developed the method using simultaneous determination of four components including geniposide, gardenoside, geniposic acid and chlorogenic acid. Against this backdrop, this study aims to propose a new calculation for gardenoside and geniposide concentrations by analyzing their concentrations in Gardeniae fructus.     

多指标综合考察巴中产栀子提取工艺

目的:多指标综合考察巴中产栀子提取工艺。方法:采用正交设计实验,考察料液比、提取次数、提取时间以及超声频率对巴中产栀子主要有效成分得率的影响,用高效液相色谱仪结合紫外检测器测定栀子提取液中栀子苷、西红花苷Ⅰ的含量,用高效液相色谱仪结合蒸发光散射检测器测定熊果酸含量。结果:用水提取巴中产栀子主要有效成分栀子苷最佳提取方案为料液比1∶15,提取3次,每次提取15 min,100 kHz频率超声提取;熊果酸的最佳提取方案为栀子原粉按栀子苷最佳得率方案提取后的药渣,用乙醇超声提取,料液比为1∶10,提取2次,每次提取60 min,100 kHz频率超声提取。应用统计软件,建立提取次数、提取时间、超声频率与Z总分之间多元非线性拟合回归方程如下Y=2.871 864 X12+0.002 283 X22-0.824 94X32+0.035 945 X1X2+0.702 867 X1X3-0.126 25 X2X3-13.271 6 X1+0.017 6 X2+8.144 655 X3,R=0.999 9。结论:采用多指标综合考察巴中产栀子提取工艺,指标全面,方法客观,通过验证性试验证明工艺稳定,值得推广。     

越鞠胶囊中香附、栀子TLC鉴别和栀子苷含量测定研究

目的:建立越鞠胶囊中香附、栀子的TLC定性鉴别法和栀子苷的高效液相色谱含量测定法。方法;以α-香附酮为对照品,采用正己烷-醋酸乙酯(9:1)为展开剂,在UV254nm下检视,和以栀子苷为对照品,采用氯仿-甲醇(3:1)为展开剂,香草醛硫酸试液为显色剂,分别对越鞠胶囊中香附和栀子进行薄层色谱法定性鉴别。采用Hpersil C_(18)柱(4.6mm×250mm,5μm),甲醇-水(25:75)为流动相,在238nm检测波长下,以HPLC法测定了越鞠胶囊中栀子苷的含量。结果:越鞠胶囊薄层色谱中,α-香附酮和栀子苷斑点清晰,阴性对照无干扰,并改进了药典中定性鉴别方法的某些缺陷。HPLC定量分析中,栀子苷线性范围为 0.30～1.50 μg(r=1.000),平均回收率为103.6％,RSD=1.0％。方法灵敏度高,结果准确,重现性好。结论:分析方法简便可行,可用于该制剂的质量控制。     

HPLC同时测定栀子药材中栀子苷和西红花苷-1的含量

目的同时测定10批栀子药材中栀子苷和西红花苷-1的含量。方法采用RP-HPLC法,ShimpackVP-ODS柱,乙腈-水梯度洗脱,检测波长238nm(0～20min,检测环烯醚萜苷类)、440nm(20～60min,检测西红花苷类)。结果和结论该方法简便、准确、重复性好,可同时测定栀子中不同检测波长的两大类有效成分。     

Metabolic profile of Fructus Gardeniae in human plasma and urine using ultra high-performance liquid chromatography coupled with high-resolution LTQ-orbitrap mass spectrometry

1. In China, Fructus Gardeniae was used as a traditional Chinese medicine (TCM) with a wide array of biological activities. The bioactive components identified in Fructus Gardeniae mainly included iridoids, flavonids, pigments, and so on. Among them, iridoids were regarded as important compounds in Fructus Gardeniae. Though analyses of the constituents in biological samples after oral administration of Fructus Gardeniae effective fraction or its active compounds have been reported, few efforts have been made to investigate the metabolic profile of Fructus Gardeniae in humans. In this study, the constituents and metabolites of Fructus Gardeniae in human blood and urine after oral administration of Fructus Gardeniae were investigated using ultra high-performance liquid chromatography (UHPLC) coupled with high-resolution LTQ-Orbitrap mass spectrometery.

2. Totally, 14 constituents (two parent compounds and 12 metabolites) of Fructus Gardeniae were identified in human plasma and urine either by comparing the retention time and mass spectrometry data with that of reference compounds or by the accurate high-resolution MS/MS data of the chemicals. The compounds identified were mainly iridoid glycosides such as geniposide and the derivatives of genipin-O-glucuronide. Among them, 11 metabolites were detected in human plasma and urine while the other three metabolites including geniposidic acid (M1), demethylation derivative of genipin-O-glucuronide (M2), and dehydration product of mono-hydroxylated genipin-O-glucuronide (M9) were only discovered in human urine. Further, the possible metabolic pathways of Fructus Gardeniae in vivo were proposed and the peak area–time curve of the most abundant metabolite genipin-O-glucuronide (M13) in human plasma after oral administration of Fructus Gardeniae was depicted. The results suggested that a metabolic difference existed between rats and humans.

3. The results obtained in the present research would provide basic information to understand the metabolic profile of Fructus Gardeniae in humans and explore the chemicals responsible for the hepatotoxicity of Fructus Gardeniae in vivo. Moreover, it would be beneficial for us to further study the pharmacokinetic behavior of Fructus Gardeniae in humans systematically.     

消渴健脾胶囊质量标准研究

目的 建立消渴健脾胶囊的质量标准.方法 采用显微镜鉴别制剂中直接以粉末入药的白术、葛根、大黄、茯苓、车前子5味中药材的显微特征;采用薄层色谱(TLC)法定性鉴别栀子、土茯苓、大黄、茯苓、莱菔子、葛根6味药材的特征斑点;采用高效液相色谱(HPLC)法测定制剂中栀子苷的含量,色谱柱为Cosmosil C18柱(250 mm...