复方丹参滴丸辅助治疗2型糖尿病65例

目的观察复方丹参滴丸辅助治疗2型糖尿病的临床效果。方法选择2型糖尿病患者130例,随机均分为对照组和治疗组各65例,对照组口服格列齐特缓释片(80 mg,每日2次)、阿卡波糖片(100 mg,每日3次)。治疗组在对照组基础上加服复方丹参滴丸(10丸,每日3次),疗程10周。结果对照组总有效率为60.00%,治疗组总有效率为81.54%,两组总有效率比较有显著性差异(χ2=5.46,P<0.05);两组治疗10周后空腹血糖、餐后2 h血糖、糖化血红蛋白、血清总胆固醇和甘油三酯均显著下降,且治疗组改善更明显。结论复方丹参滴丸辅助治疗2型糖尿病疗效较好,值得临床推广。     

采用高效液相色谱法同时测定复方丹参滴丸中的多成分含量

目的:采用高效液相色谱法(HPLC法)同时测定复方丹参滴丸中的7种成分.方法:应用Diamonsil C18色谱柱,以乙腈-甲醇-0.1%磷酸溶液为流动相进行梯度洗脱,在柱温35 ℃下使用205、270和285 nm三波长同时检测.结果:7种成分的峰面积与浓度的线性关系良好,平均回收率在94.3%～101.3%间,加样...     

Improved quality control method for Danshen products--consideration of both hydrophilic and lipophilic active components

The current study intends to provide an improved quality control analysis for Danshen product-a representative herbal product with known active components that are both hydrophilic and lipophilic in nature. A simple HPLC method with photodiode-array (PDA) ultraviolet detection was developed for the simultaneous determination of three major lipophilic components (cryptotanshinone, tanshinone I and tanshinone IIA) and three major hydrophilic components (danshensu, protocatechuic aldehyde and salvianolic acid B) of Danshen (Salvia miltiorrhiza). These six components were successfully separated using Radial-pak C18 cartridge with the elution gradient consisting of 0.5% acetic acid in water and 0.5% acetic acid in acetonitrile at a flow rate of 1 ml/min. The intra-day and inter-day precisions of the analysis were within 2.32 and 2.0%, respectively. The detection limits were 0.02, 0.01, 0.01, 0.05, 0.005 and 0.02 microg/ml for cryptotanshinone, tanshinone I, tanshinone IIA, danshensu, protocatechuic aldehyde and salvianolic acid B, respectively. The developed method has been applied to the simultaneous determination of above six major components in Fufang Danshen Tablet and Dripping Pill products by extraction with methanol and water. It has been demonstrated that salvianolic acid B and danshensu are the major components among the eight commercial Fufang Danshen products studied. The current developed method with methanol as extraction solvent provides a simple and efficient method for simultaneous detection of both lipophilic and hydrophilic major components in Danshen products.     

复方丹参滴丸治疗糖尿病视网膜病变的临床效果及安全性评价

目的 探讨复方丹参滴丸对糖尿病视网膜病变的临床治疗效果.方法 整理我院86例糖尿病视网膜病变患者的临床资料,在治疗当中随机分为治疗组和对照组各43例,治疗组患者使用复方丹参滴丸,对照组使用羟苯磺酸钙胶囊进行治疗,完成治疗后对患者的临床治疗效果进行比较分析,观察不同药物情况下患者的治疗疗效差异.结果 治疗组患者的临床效果明显高于对照组,(P<0.05),在患者的临床检查结果当中,患者的症状情况改善明显.结论 在糖尿病视网膜病变患者的治疗过程中,可以使用复方丹参滴丸治疗,临床治疗效果明显,且患者的药物使用安全性较高,在临床当中可以推广使用.     

复方丹参滴丸对华法林在人体内药动学和药效学的影响

目的研究复方丹参滴丸对华法林在人体内药动学和药效学的影响,以及单独服用复方丹参滴丸4周后对凝血酶原时间(PT)和活化部分凝血活酶时间(APTT)的影响。方法采用随机、单盲、双周期交叉、安慰剂对照试验设计。12名男性健康志愿者随机分为2组(6人/组),连续5周每日分别服用复方丹参滴丸(10片,每天3次)或安慰剂(10片,每天3次);d29口服单剂量华法林5 m g;第2周期2组交叉服用安慰剂或复方丹参滴丸,其余给药方案不变。按要求收集志愿者血样,分别以高效液相色谱法(H PLC)测定华法林的血药浓度以及半自动血凝仪测定常见凝血指标。结果合用复方丹参滴丸后,华法林的药动学参数cmax、AUC0~144、AUC0~∞、t1/2显著增加(P<0.05),CL/F显著减小(P<0.05),tmax和V/F没有显著变化;华法林的药效学参数发生显著变化。单独服用复方丹参滴丸4周后,PT和APTT均发生显著变化。结论复方丹参滴丸可影响华法林的药动学和药效学;单独服用复方丹参滴丸4周对凝血功能有显著影响。     

5种复方丹参口服制剂质量标准对比分析与启示

目的:对比5种复方丹参口服制剂质量标准的异同,分析日用量含饮片量与活性组分含量,为临床用药综合评估提供参考.方法:从《中华人民共和国药典》2020年版提取这5种制剂的处方、制法、鉴别、检查及含量测定指标,结合用法用量计算日用量相当于饮片量及活性组分量,分析其异同.结果:复方丹参滴丸与其他4种制剂组方相似,但处方中君药丹...     

丹参中丹参酮成分的HPLC-MS(n)研究

目的研究丹参中丹参酮成分的ESI-MS（n）规律,建立其HPLC-MS（n）特征图谱。方法以丹参酮ⅡA为代表,初步探讨丹参酮成分的ESI-MS（n）规律。应用HPLC-MS（n）,ESI（＋）模式,以水-乙腈为流动相,检测波长254 nm,梯度洗脱绘制丹参中丹参酮成分的特征图谱。结果得出丹参酮成分的ESI-MS（n）可能的裂解途径,得到其HPLC-MS（n）特征图谱,对特征图谱中11种主要化合物进行了精确归属。结论丹参酮类成分具有相似的ESI-MS（n）行为,根据质谱提供的各流份的分子量信息及多级质谱的裂解信息,可用于鉴别丹参酮类成分。所得到的丹参中丹参酮成分的MS（n）TIC图,可用于丹参药材中丹参酮类成分的指纹鉴别。     

银丹心脑通软胶囊治疗冠心病心绞痛气滞血瘀证临床观察

目的:观察银丹心脑通软胶囊对冠心病心绞痛的疗效及不良反应。方法:采用随机对照研究方法,与复方丹参滴丸进行对照,共观察病人60例,治疗组30例,对照组30例。结果:银丹心脑通软胶囊治疗组治疗心绞痛总有效率为83.3%,心电图疗效为53.3%,中医症状总有效率为86.7%;复方丹参滴丸对照组疗效分别为80.0%、46.7%、80.0%。两组间比较,无显著性差异。结论:银丹心脑通软胶囊对冠心病心绞痛气滞血瘀证有较好疗效。     

复方丹参滴丸治疗冠心病心绞痛60例疗效观察

目的探讨复方丹参滴丸治疗冠心病心绞痛的疗效,评价其用药的合理性和安全性。方法选取符合条件的冠心病心绞痛患者100例,随机分为治疗组和对照组,分别为60例和40例。治疗组用复方丹参滴丸,对照组用甘油三酯片,疗程均为60天,于治疗前后分别做心绞痛症状改善、心电图疗效和血液流变学等的连续观察。结果治疗组和对照组心绞痛症状改善的总有效率分别为88．3％和60．0％。心电图疗效改善的总有效率分别为71．7％和52．5％。治疗组明显高于对照组,差异有显著性。血液流变学指标的比较显示,治疗组在改善全血黏度的高切和低切,毛细管血浆黏度,红细胞压积,纤维蛋白原等方面均较对照组明显。结论复方丹参滴丸在治疗冠心病心绞痛方面效果明显。     

复方丹参联合依那普利治疗老年冠心病心力衰竭66例

目的 观察复方丹参滴丸联合依那普利治疗老年冠心病心力衰竭的临床疗效.方法 选择符合我国冠心病慢性心力衰竭标准的患者66例,采用复方丹参滴丸联合依那普利治疗,疗程15周,治疗前后分剐用超声心动图测定左室射血分数(LVEF)、心排血量(CO)、E/A比值、左室舒张朱期内径(LVEDD),6 min步行耐量试验(6MWT)以及24 h动态血压检测等指标.结果 66例患者治疗后,心功能和运动耐量、动态血压实验检测均有明显改善,治疗前后血脂指标各参数间比较差异有明显统计学意义(P＜0.05＝.结论 该中西结合方案在治疗老年冠心病心力衰竭上能显著改善心功能、提高患者生活质量,适合老年患者应用.     

Identification of phenolic compounds in rosemary honey using solid-phase extraction by capillary electrophoresis-electrospray ionization-mass spectrometry

Complex extracts of rosemary honey constituents often require very effective separation techniques to allow the identification of different compounds. Capillary electrophoresis (CE) coupled to mass spectrometry (MS) detection can provide structure-selective information about the analytes in such matrices and has turned out to be an attractive alternative to HPLC methods. A simple and cost-effective analytical method involving solid-phase extraction (SPE) and capillary zone electrophoresis coupled to electrospray ionization-ion trap mass spectrometry (CZE-ESI-MS) to identify and characterize phenolic compounds in rosemary honey is described. The SPE, CE and ESI-MS parameters were optimized in order to maximize the number of phenolic compounds detected and the sensitivity of their determination. All CE–ESI-MS experiments were performed with uncoated fused-silica capillaries and an alkaline volatile buffer system consisting of 100 mM NH₄Oac with 10% of 2-propanol at pH 10. Since sheath liquids can made significant effects on the sensitivity in typical CE–ESI-MS application, the effect of type and flow rate of the sheath liquid on the sensitivity of phenolic compounds were investigated. As result, the best sensitivity was obtained with a sheath liquid containing 2-propanol/water 60:40 (v/v) and 0.1% (v/v) of triethylamine at 3 μL/min in the negative ion mode. We describe the first method for the analysis of phenolic compounds in rosemary honey at mg/L levels by using a simple SPE before CE–ESI-MS analysis.     

Radioimmunoassay and gas chromatography/mass spectrometry for a novel antiglaucoma medication of a prostaglandin derivative,S-1033, in plasma

A radioimmunoassay (RIA) and a gas chromatographic/mass spectrometric (GC/MS) method for a new antiglaucoma medicament, the prostaglandin derivative sodium (5Z,9α,11α,13E)-9,11-dihydroxyprosta-5,13-dienoate (S-1033), in human and rabbit plasma were investigated. For a competitive RIA, antisera from rabbit and radioiodine-labeled S-1033 were prepared by immunizing a conjugate of S-1033 with bovine serum albumin and by the Bolton and Hunter method, respectively. Pretreatment by C₁₈ solid-phase extraction (SPE) for rabbit plasma sample and further purification by high-performance liquid chromatography (HPLC) for human plasma samples followed by the RIA (SPE/RIA and HPLC/RIA, respectively) were developed. The assay recoveries of SPE/RIA and HPLC/RIA were both excellent and the limits of quantitation were 320 and 10 pg ml⁻¹, respectively. GC/MS for plasma samples after solid-phase extraction and thin-layer chromatographic purification was also developed using deuterium-labeled S-1033 as internal standard. The limit of quantitation was 100 pg ml⁻¹ in human or rabbit plasma. Rabbit plasma samples after administration of this drug were measured by SPE/RIA and GC/MS and the assay results from both methods agreed well. The SPE/RIA, HPLC/RIA and GC/MS assay methods were suitable for measuring samples from preclinical studies, clincial studies and cross-validation, respectively.     

复方丹参滴丸对急性心肌梗死大鼠基因表达谱的影响

目的：利用基因芯片技术对复方丹参滴丸对心肌梗死大鼠基因表达的影响进行评价和研究。方法：使用冠脉结扎法造成大鼠心肌缺血模型,并提取给药组和模型组大鼠心肌缺血区组织的总RNA,用大鼠全基因组芯片分析其基因组表达谱变化。结果：基因芯片结果显示,与模型组相比,给药组表达量发生变化的基因（Ratio〉2或〈0．5）有49条,其中表达下调的有39条,主要有Ppp3r1、Rhoa和Nppa,表达上调的有10条,包括H2,T24、RT1-CE15、Ptprb和Hcst等。结论：复方丹参滴丸可通过调节Wnt信号通路等多个基因和信号途径来减小心肌梗死模型大鼠心脏缺血区的心肌损伤。     

Chemical fingerprint and metabolic fingerprint analysis of Danshen injection by HPLC-UV and HPLC-MS methods

HPLC–UV and HPLC–MS techniques were used in fingerprint analysis of Danshen injection and its raw materials (roots and rhizoma of Salvia miltiorrhiza). HPLC profiles of Danshen injections from a Chinese pharmaceutical factory and their raw materials were established as their characteristic fingerprint and employed to assess their consistency and difference. To develop the representative fingerprint of Danshen injection, 10 batches of samples were analyzed under the same HPLC conditions. The results showed that 10 batches of Danshen injections had very similar HPLC fingerprints. To characterize the major constituents of Danshen injection for quality control, 11 major chromatographic peaks were characterized by their MS spectra and comparison with the reference standards. Through comparison of the HPLC profiles of Danshen injection with its raw material, it was found that they are greatly different, which indicated the changes of major constituents in the course of preparation procedure. In addition, the rat's plasma was analyzed by HPLC–MS technique after intravenous administration of Danshen injection at different time intervals to explore the in vivo metabolism of the major active constituents. Except for protocatechuic aldehyde, the major phenolic acids in Danshen injection appeared in rat's plasma after intravenous administration, but quantity of each phenolic acids was very different from that in Danshen injection. With the administration time prolonged danshensu and salvianolic acid B disappeared quickly, salvianolic D, lithospermic acid and salvianolic A slowly decreased and maintained relatively high concentration after 30 min of intravenous administration. This indicated that polyphenolic acids were significant for biological acitivity of Danshen injection. It might be concluded that chemical fingerprint combined with metabolic fingerprint is a useful means to control the quality and to clarify the possible mechanism of action of herbal products.     

Hplc/electrospray ionization mass spectrometric analysis of the heterocyclic aromatic amine carcinogen 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine in human milk

A new procedure has been developed for the extraction of 2-amino-1-methyl-6-phenyl-imidazo[4,5-b]pyridine (PhIP) and other heterocyclic aromatic amines from human breast milk samples. Extracts were analyzed by high-performance liquid chromatography/electrospray ionization/tandem mass spectrometry (HPLC/ESI-MS/MS) with selective reaction monitoring detection. Tandem ESI-MS/MS detection provides much improved sensitivity and specificity, compared with those of a previous method that used selected ion monitoring. Milk samples were collected from 48 healthy volunteers, including five vegetarians. Donors completed a detailed dietary questionnaire. The concentrations of PhIP in the milk samples were low and below the limit of quantification (0.68 pg/mL) for all subjects except one, for whom a concentration of 1.0 pg PhIP/mL was measured. Our results indicate that the levels of PhIP in human milk are substantially lower than what was previously reported.     

Determination of digoxin in human serum using stable isotope dilution liquid chromatography/electrospray ionization-tandem mass spectrometry

A method for the determination of digoxin in human serum using a liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) technique is reported. Digoxin and the internal standard, [21,21,22-(2)H(3)]digoxin, were extracted from 250 mul of human serum using a solid phase extraction cartridge (Oasis HLB) and analyzed by LC/ESI-MS/MS in the selected reaction monitoring mode. The intra- and inter-assay reproducibility and accuracy were satisfactory within the quantification range of 0.20-3.20 ng/ml. The concentrations of digoxin in the serum samples obtained from digitalized patients (n=19) were in the range of 0.25-2.84 ng/ml, which were compared to those obtained by radioimmunoassay.     

透骨草总皂苷的提取与含量测定

目的研究透骨草总皂苷的提取方法及含量测定。方法采用正交实验法优化透骨草总皂苷乙醇回流提取法最佳提取工艺,同时采用HPLC法测定总皂苷含量。结果正交实验确定总皂苷最优提取条件:70%乙醇提取2次,每次1h,溶剂用量为12倍量。HPLC法测定透骨草总皂苷含量(原药材中含量)达到2.71%。结论乙醇回流提取法为透骨草总皂苷最佳提取方法,HPLC法测定总皂苷含量简便、可行、精确。     

Characterization and quantitative analysis of DNA adducts formed from lower chlorinated PCB-derived quinones

Polychlorinated biphenyls are wide pollutants readily detected in environmental and human specimens. DNA adduction occurs through the corresponding quinones. Polychlorinated biphenyls are first metabolized to arene oxides, which can be further oxidized to dihydroxy metabolites by microsomal cytochrome p450s. The catechol and hydroquinone products are further oxidized by peroxidases to quinones, which are electrophilic and capable of reacting with DNA to form adducts. DNA adduction is initiated by Michael addition preferentially to guanosine followed by stabilization through enolization. Another nucleophilic attack forms a five-membered ring, which aromatizes by dehydration to form the final adduct. This report describes the characterization and quantitative study of DNA adducts formed from lower chlorinated PCB-derived quinones. Quantitative study by HPLC/ESI-MS/MS and (32)P-postlabeling-HPLC gave the adduct levels in the range of 3-1200 adducts per 10(8) nucleotides. These results demonstrate that increasing chlorine substitution is associated with lower yields of DNA adduct. Although (32)P-postlabeling is more sensitive than HPLC/ESI-MS/MS for the quantitative analysis of DNA adducts, modification levels were severely underestimated by the (32)P-postlabeling assay as compared to the HPLC/ESI-MS/MS assay.     

Characterization of impurities in semi-synthetic vinorelbine bitartrate by HPLC-MS with mass spectrometric shift technique

A simple and sensitive method of high-performance liquid chromatography coupled with electrospray ionization mass spectrometry (HPLC/ESI-MS) was developed to separate and identify impurities in semi-synthetic vinorelbine bitartrate sample. The analytical HPLC was carried out on a reversed-phase C8 column using 0.02 M ammonium formicate buffer (pH 4.2) and methanol (46:54, v/v) as mobile phase at a flow rate of 0.8 ml/min at room temperature and a UV detection at 267 nm. The on-line HPLC/ESI-MS/MS was performed using ion trap analyzer in positive ion mode. Applying mass spectrometric shift technique to HPLC/ESI-MS/MS analysis, four impurities were identified as 18'-O-demethylvinorelbine (impurity-1), 6'-N-methylvinorelbine (impurity-2), 23-O-demethylvinoreline (impurity-3) and 17-bromovinorelbine (impurity-4), respectively, in investigated vinorelbine bitartrate sample. The four impurities, in which the impurity-1 was not reported as the semi-synthetic process impurity for vinorelbine bitartrate elsewhere, were isolated by preparative high-performance liquid chromatography. Their structures were further confirmed by means of 1D and 2D NMR spectra. Structural elucidation by spectral data was discussed.     

HPLC测定复方丹参片中三七总皂苷的含量

目的建立复方丹参片中三七有效成分的含量测定方法。方法采用HPLC法测定本品中三七中人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1的含量。结果人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1线性范围分别依次为0.850～8.524、0.922～9.013、0.377～3.317μg;平均回收率分别为101.1%、101.2%、103.2%,RSD分别为1.5%、1.6%、1.8%。结论本方法简便可靠,结果稳定,可用于丹心舒胶囊中三七的有效成分的含量测定。