近红外光谱技术快速测定杞菊地黄丸中马钱苷的含量

目的应用近红外光谱技术建立杞菊地黄丸(浓缩丸)中马钱苷含量的快速测定方法。方法以HPLC法测定样品中马钱苷的含量作为参考值,同时使用近红外漫反射光谱技术,采集113份杞菊地黄丸样品的近红外漫反射光谱,利用偏最小二乘法,建立马钱苷含量的快速测定模型。结果建立的校正模型的相关系数和内部交叉验证均方差分别为0.998 8和0.093 4;经外部验证,模型的预测相关系数r和预测均方差分别为0.986 7和0.084 9。结论该方法操作简便,结果准确、可靠,可用于杞菊地黄丸中马钱苷含量的快速测定。     

阿立哌唑粉末近红外光谱定量模型的建立与应用

目的 建立阿立哌唑粉末近红外光谱定量模型，探讨近红外光谱技术监测阿立哌唑原辅料混合终点的同时预测粉末中阿立哌唑含量的可行性。方法 采集含量范围在84.60%～112.8%内的阿立哌唑粉末样品的近红外光谱，使用高效液相色谱法测定样品的实际含量，选择多元散射校正结合Savitzky-Golay卷积平滑的预处理方法，建模波段为5 550.00～7 400.00 cm^-1,使用偏最小二乘法建立含量定量模型。使用建立的模型分别预测离线样品和经过光谱校正的在线样品，并用HPLC法测定的含量进行验证。结果 模型校正均方根误差为2.94,校正相关系数为0.955 2。离线样品的预测均方根误差为4.82,在线样品的预测均方根误差为3.34,离线样品和在线样品的预测结果与HPLC法测定的结果一致(P>0.05)。结论 建立的基于近红外光谱技术的阿立哌唑粉末定量模型在监测阿立哌唑原辅料混合终点的同时可在线准确预测粉末中阿立哌唑的含量。     

近红外漫反射光谱快速检测川贝母中浙贝母的掺入量

目的：应用近红外漫反射光谱技术和化学计量学方法，建立一种快速检测川贝母中浙贝母掺人量的新方法。方法：以含不同川贝母和浙贝母比例的41个样本建立校正集，采集其近红外漫反射光谱数据，通过偏最小二乘法进行回归，经内部交叉验证，建立校正模型，进而对预测集样品进行分析。结果：对6个预测集样本进行预测分析，得到近红外光谱预测值与真值的相关系数r=0．9997，样品回收率为97．96％-100．9％，RSD为0．81％。结论：本方法具有快速方便、结果准确的特点，可以应用于外观相似，化学成分相近的中药材的品质分析和质量控制。     

近红外光谱法快速检测维C银翘片中维生素C的含量

目的 应用近红外漫反射技术和化学计量学方法对维C银翘片中的维生素C进行快速定量分析.方法 采集样品的近红外漫反射光谱数据,采用偏最小二乘法(PLS)建立光谱数据和样品中维生素C含量的相关模型,应用所建模型对未知样品进行预测.结果 应用维生素C定量分析模型,以731个维C银翘片样品为校正集,浓度范围为86～ 201mg·...     

近红外光谱技术快速测定杞菊地黄丸的水分含量

目的应用近红外光谱技术建立一种杞菊地黄丸(浓缩丸)中水分含量的快速测定方法。方法以甲苯法测定的样品中水分的含量为真实值,运用近红外漫反射光谱技术采集96份杞菊地黄丸(浓缩丸)样品的近红外漫反射光谱,结合偏最小二乘法(PLS)建立水分含量的定量分析模型。结果所建水分校正模型的相关系数(R2)和内部交叉验证均方差(RMSECV)分别为0.988 09和0.0587;经外部验证,模型的预测相关系数(r2)和预测均方差(RMSEP)分别为0.9969和0.075 2。结论该方法操作简便,无污染,结果准确可靠,可用于杞菊地黄丸(浓缩丸)中水分含量的快速测定。     

偏最小二乘-近红外漫反射光谱法测定还原型谷胱甘肽片

采集还原型谷胱甘肽片(素片)的近红外漫反射光谱,以HPLC测定结果为参考值,运用偏最小二乘法(PLS)建立含量预测模型.所建模型的交叉验证均方根误差(RMSECV)为0.024 13,预测均方根误差(RMSEP)为0.008 57,预测集的相关系数(R)为0.972 54,证明近红外漫反射光谱法结合多元分析技术可快速测定还原型谷胱甘肽片的含量,并可望用于生产过程控制.     

近红外光谱法快速测定罗布麻叶中总黄酮含量

目的建立罗布麻叶中总黄酮含量近红外光谱定量分析模型,快速测定罗布麻叶中总黄酮含量。方法采集并用多种预处理近红外光谱,结合偏最小二乘法(PLS),建立罗布麻叶中总黄酮含量的定量分析模型并对所建立的模型进行优化。结果优化后定量模型的校正集预测值与测定值之间的相关系数RC为0.979 6,校正集标准差(SEC)为0.21,验证集标准差(SEP)为0.13、交互检验验证集标准差(SECV)为0.27。结论该定量模型具有较高的预测效果,建立的方法可快速定量分析罗布麻叶中总黄酮含量。     

NIRDRS法对微球制剂的粒径及跨度的研究

目的：采用近红外漫反射光谱技术，建立一种快速测定微球的粒径及其跨度的方法。方法：建立校正样品集与测试样品集。采集近红外光谱，运用偏最小二乘法建立数学模型。对测试集进行预测。结果：校正样品集的最佳主成分数分别为(Rank1)=2，(Rank2)=1；内部交叉验证均方差(RMSECV1)=0．78，(RMSECV2)=0．22；决定系数(R^21)=98．58。(R^22)=93．35。测试样品集的预测结果，粒径：预测均方差(RMSEP)=0．99，决定系数(R^2)=97．84，评估均方差(RMSEE)=1．12；跨度：预测均方差(RMSEP)=0．28。决定系数(R^2)=93．03，评估均方差(RMSEE)=0．23。结论：近红外漫反射光谱测定微球的粒径及其跨度结果可靠，可用于微球制剂的质量控制。     

近红外光谱法测定盐酸吡格列酮片的含量

目的：利用近红外光谱建立快速测定盐酸吡格列酮片含量的方法。方法：用HPLC法测定100批盐酸吡格列酮片样品含量并采集各样品的近红外光谱数据,从中随机抽取80批样品组成校正集,另20批样品组成测试集,采用偏最小二乘法（PLS）建立定量模型,并预测测试集样品的盐酸吡格列酮含量。结果：所建立定量模型的交叉验证测定系数r^2为0．9903,交叉验证均方差（RMSPCV）为0．394;测试集样品的测定系数r^2为0．9875,预测均方差（RMSEP）为0．259,平均预测偏差0．18％。结论：本法操作简便、快速、环保,可用于盐酸吡格列酮片的快速定量分析。     

近红外漫反射光谱-偏最小二乘法非破坏测定复方氨酚烷胺片

本文应用偏最小二乘法(PLS)同近红外漫反射光谱相结合，对复方氨酚烷胺片进行了无损非破坏定量分析，以样品中对乙酰氨基酚和盐酸金刚烷胺为活性成分建立了最佳的数学校正模型。分别讨论了常规光谱和二阶导数光谱中主成分数对PLS定量预测能力的影响，预测了未知样品。     

Identification of kaempferol as a monoamine oxidase inhibitor and potential Neuroprotectant in extracts of Ginkgo biloba leaves

The effects of Ginkgo biloba leaf extract on rat brain or livermonoamine oxidase (MAO)-A and -B activity, biogenic amine concentration in nervous tissue, N-methyl-D-aspartate (NMDA)- and N-(2-chloroethyl)-N-ethyl-2-bromobenzylamine (DSP-4)-induced neurotoxicity and antioxidant activity was investigated to determine the effects of the extract on monoamine catabolism and neuroprotection. Ginkgo biloba leaf extract was shown to produce in-vitro inhibition of rat brain MAO-A and -B. The Ginkgo biloba extract was chromatographed on a reverse-phase HPLC system and two of the components isolated were shown to be MAO inhibitors (MAOIs). These MAOIs were identified by high-resolution mass spectrometry as kaempferol and isorhamnetin. Pure kaempferol and a number of related flavonoids were examined as MAOIs in-vitro. Kaempferol, apigenin and chrysin proved to be potent MAOIs, but produced more pronounced inhibition of MAO-A than MAO-B. IC50 (50% inhibition concentration) values for the ability of these three flavones to inhibit MAO-A were 7 x 10(-7), 1 x 10(-6) and 2 x 10(-6) M, respectively. Ginkgo biloba leaf extract and kaempferol were found to have no effect ex-vivo on rat or mouse brain MAO or on concentrations of dopamine, noradrenaline, 5-hydroxytryptamine and 5-hydroxyindoleacetic acid. Kaempferol was shown to protect against NMDA-induced neuronal toxicity in-vitro in rat cortical cultures, but did not prevent DSP-4-induced noradrenergic neurotoxicity in an in-vivo model. Both Ginkgo biloba extract and kaempferol were demonstrated to be antioxidants in a lipid-peroxidation assay. This data indicates that the MAO-inhibiting activity of Ginkgo biloba extract is primarily due to the presence of kaempferol. Ginkgo biloba extract has properties indicative of potential neuroprotective ability.     

高效液相色谱法测定银杏叶提取物及其制剂中银杏酸的含量高效液相色谱法测定银杏叶提取物及其制剂中银杏酸的含量

目的建立银杏叶提取物及其制剂中银杏酸含量的HPLC测定方法。方法银杏叶提取物及其制剂经石油醚提取，提取液浓缩后用石油醚定容，HPLC直接测定，并用LC/MS对其中的银杏酸进行了定性鉴定。色谱分析条件：色谱柱为Inertsil ODS-2，流动相为甲醇-3% HAc溶液（92∶8），流速1.0 mL·min^-1,柱温40 ℃，紫外检测波长310 nm。结果银杏叶提取物中存在6种银杏酸C13:0，C15:0，C15:1，C17:1，C17:2和一种可能是C17∶3的银杏酸化合物，其中C13∶0，C15∶1和C17∶1占总银杏酸的94%以上。实验测得高银杏酸含量的提取物中银杏酸含量为1.12%,RSD为2.4%（N=5）；银杏叶提取物片剂中银杏酸含量为49.2 μg·g^-1,RSD为4.3%（N=5）。平均回收率98.2%，RSD为2.6%（N=5）。结论该方法准确、快速、简便，可用于银杏叶提取物及其制剂中银杏酸的定量分析。     

银杏叶片中银杏黄酮在Beagle犬体内的药动学研究

目的以槲皮素为代表,研究银杏叶片中银杏黄酮类成分在Beagle犬体内的药动学特征。方法 Beagle犬口服给药银杏叶片后,按设定时间静脉采血。血样经固相萃取、酸水解后,以HPLC-ECD测定不同时间点血浆中槲皮素的浓度。应用DAS数据处理软件对数据进行统计学处理。结果口服给药后,槲皮素在Beagle犬体内的药动学过程符合二房室模型,其主要药动学参数为t1/2z5.67 h,AUC0-t63.8 g.L 1.h,Cmax15.9 g.L 1。结论建立的方法简单、灵敏、准确,可用于研究以槲皮素为代表的银杏黄酮类成分的药动学特征,为银杏叶片的临床应用提供了依据。     

Analysis of ginkgolides and bilobalide in Ginkgo biloba L. extract injections by high-performance liquid chromatography with evaporative light scattering detection

A RP-HPLC method with evaporative light scattering detection (ELSD) was developed for the determination of ginkgolides and bilobalide in Ginkgo biloba L. extract injections. The samples were extracted with ethyl acetate and the resulting extract was purified by aluminum oxide column. The resultant solution was determined by HPLC on a C(18) column with methanol-water (33:67, v/v) as eluent. The optimum ELSD parameters were set. The recovery of the method was between 98.3 and 102.1%. The method is suitable for routine quantitation of terpenes in Ginkgo biloba L. extract injections.     

银杏叶提取物对糖尿病纤溶酶原激活物抑制物1及凝血噁烷B2影响

目的 :观察银杏叶提取物对 2型糖尿病病人纤溶酶原激活物抑制物 1(PAI 1)及凝血烷B2(TXB 2 )的影响。方法 :将 6 4名 2型糖尿病病人随机分为常规治疗组和银杏叶提取物治疗组各 32例 ,正常对照组 30例。银杏叶提取物治疗组在常规治疗基础上 ,予银杏叶提取物注射液 2 0mL +氯化钠注射液 2 5 0mL ,iv ,gtt ,qd。2 1d后检测空腹和餐后 2h血糖、空腹胰岛素 (FINS) ,PAI 1,TXB 2。结果 :银杏叶提取物治疗组血浆FINS ,PAI 1及TXB 2在治疗后显著下降 ,下降值分别为 (16±s 6 )mU·L- 1,(33± 6 ) μg·L- 1,(73± 12 )ng·L- 1(P <0 .0 1)。结论 :银杏叶提取物可以降低血浆FINS ,PAI 1及TXB 2的水平 ,对预防 2型糖尿病的大血管病变具有一定作用     

HPLC法快速测定银杏叶中银杏总黄酮醇苷含量

目的建立银杏叶中特征性成分总黄酮醇苷的快速含量分析方法,比较不同的采集地总黄酮醇苷含量差异。方法采用Alltima C18色谱柱(5μm,4.6×150mm);流动相为甲醇-0.4%磷酸(50∶50);检测波长为360nm;流速为1.0mL/min;柱温为30℃。结果Q在0.06～0.60μg范围内线性关系良好(r=0.9998);K在0.06～0.06μg范围内线性关系良好(r=0.9998);I在0.04～0.40μg范围内线性关系良好(r=0.9999)。平均加样回收率为97.6%(n=6),RSD为1.22%,银杏总黄酮醇苷的含量为0.4857%～0.8869%。结论不同产地银杏叶中总黄酮醇苷含量差异较大,该方法准确、简便,重现性好,为银杏叶质量评价提供简便快捷的方法。     

复方银杏通脉胶囊的研制

目的：研究复方银杏通脉胶囊的制备和质量标准。方法：用两种深度乙醇提取银杏叶活性成份;建立薄层色谱法鉴别法,正丁醇提取物含量控制成品质量。结果：银杏叶活性成春分 较高,薄层色谱法专属性强,正丁醇提取物不低于１２ｍｇ／粒,ＲＳＤ为１．０４％,重现性好。结论：制备工艺合理,所得制剂质量可控,性质稳定,可满足临床用药需求。     

银杏酸的高效液相色谱法测定

目的建立银杏酸的简便预净化处理和HPLC含量测定方法。方法用LC/DAD/ESI/MS对银杏酸进行定性鉴定。银杏叶经正己烷提取、硅胶柱色谱净化处理,HPLC测定。色谱分析条件:色谱柱为Inertsil ODS-2,流动相为甲醇-3% HAc溶液(92∶8),流速1.0 mL·min^-1,柱温40℃,紫外检测波长310 nm。结果银杏叶中存在5种银杏酸C13∶0,C15∶0,C15∶1,C17∶1和C17∶2,其中C15∶1和C17∶1约占银杏酸的85%,C17∶2银杏酸未见国内文献报道。银杏叶提取物经硅胶柱色谱处理后,其HPLC谱中除银杏酸峰外,几无其他杂质峰。平均回收率97.0%,RSD为1.7%(N=6)。结论该方法准确、简便、可靠,可用于银杏酸的定量分析。     

北京地区2003~2013年银杏叶提取物注射液不良反应报告分析

摘 要 目的：调查北京地区银杏叶提取物注射液（金纳多）所致药品不良反应（ADR）发生情况,为临床合理用药提供参考。方法：对北京地区2003~2013年银杏叶提取物注射液ADR上报信息进行统计归类,对发生人群、ADR症状和累及器官、发生时间、合并用药情况及处理预后情况进行回顾性分析。结果：在114例不良反应报告中,老年患者的构成比大于青壮年患者,女性患者的构成比大于男性,累及皮肤及其附件损害的ADR例数最多（35例）,其次为累及神经系统、心血管系统等。ADR发生时间无规律。银杏叶提取物注射液ADR报告中存在9例合并用药现象。新的ADR 8例,无严重ADR。结论：临床应合理使用银杏叶提取物注射液,保证临床用药安全,降低药品不良反应发生风险。     

The effect of 3-month ingestion of Ginkgo biloba extract (EGb 761) on pancreatic beta-cell function in response to glucose loading in individuals with non-insulin-dependent diabetes mellitus

In the first report (Journal of Clinical Pharmacology 2000; 40:647-654), it was shown that ingestion of 120 mg of Ginkgo biloba extract (EGb 761) daily for 3 months by normal glucose-tolerant individuals caused a significant increase in pancreatic beta-cell insulin and C-peptide response, measured as the area under the curve (AUC0-->120) during a 2-hour standard (75 g) oral glucose tolerance test (OGTT). This follow-up study was designed to determine the effect of the same Ginkgo biloba treatment on glucose-stimulated pancreatic beta-cell function in non-insulin-dependent diabetes mellitus (NIDDM) subjects. In diet-controlled subjects (fasting plasma glucose [FPG], 117 +/- 16 mg/dl; fasting plasma insulin [FPI], 29 +/- 8 microU/ml; n = 6), ingestion of Ginkgo biloba produced no significant effect on the insulin AUC0-->120 (193 +/- 53 vs. 182 +/- 58 microU/ml/h, before and after ingesting Ginkgo biloba, respectively). In hyperinsulinemic NIDDM subjects taking oral hypoglycemic medications (n = 6) (FPG 143 +/- 48 mg/dl; FPI 46 +/- 13 microU/ml), ingestion of Ginkgo biloba caused blunted plasma insulin levels from 30 to 120 minutes during the OGTT, leading to a reduction of the insulin AUC0-->120 (199 +/- 33 vs. 147 +/- 58 microU/ml/h, before and after Ginkgo biloba, respectively). The C-peptide levels increased, and so the AUC0-->120 did not parallel the insulin AUC0-->120, creating a dissimilar insulin/C-peptide ratio indicative of an enhanced hepatic extraction of insulin relative to C-peptide. Thus, in pancreatic beta-cells that are already maximally stimulated, ingestion of Ginkgo biloba may cause a reduction in plasma insulin levels. Only in NIDDM subjects with pancreatic exhaustion (FPG 152 +/- 46 mg/dl; FPI 16 +/- 8 microU/ml; n = 8), who also took oral hypoglycemic agents, did Ginkgo biloba ingestion significantly increase pancreatic beta-cell function in response to glucose loading (insulin AUC0-->120 increased from 51 +/- 29 to 98 +/- 20 microU/ml/h, p < 0.0001), paralleled by a C-peptide AUC0-->120 increase from 7.2 +/- 2.8 to 13.7 +/- 6.8 (p < 0.0001). Whether this increase is due to "resuscitation" of previously exhausted islets or increased activity of only the remaining functional islets is unclear. However, not even in this group did increased pancreatic beta-cell activity cause a reduction of blood glucose during the OGTT. It is concluded that ingestion of Ginkgo biloba extract by an NIDDM subject may increase the hepatic metabolic clearance rate of not only insulin but also the hypoglycemic agents. The result is reduced insulin-mediated glucose metabolism and elevated blood glucose.