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??OBJECTIVE To explore the determination of pethidine hydrochloride injection by using Raman spectroscopy to realize in-site non-invasive inspection. METHODS CLS algorithm was used to eliminate the interference of the ampoule, correlation coefficient was used for identification, and PLS algorithm was used to establish the quantitative model. Moreover, the transfer performance of the models was investigated when used on different portable Raman instruments. RESULTS Nineteen samples of four different batches were used to verify the method. The RESULTS showed a good coincidence with reference RESULTS on both identification and quantification, and the relative deviation from HPLC method was within 5%. Meanwhile, the Raman method showed good accuracy and repeatability with relative deviation of mean and RSD value within 1% for samples from the same batch. The differences between instruments were controlled by the key index, and quantitative analysisRESULTS of 51 samples measured on three instruments all fell in the range of 90% to 110%, among which 96% fell in a more narrow range of 95% to 105%. CONCLUSION The Raman method established in this study could be used for the in-situ non-invasive determination of pethidine hydrochloride injection.     

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??OBJECTIVE To study the chemical constituents of Erigeron annuus (L.) Pers.. METHODS The compounds were isolated and purified by Diaion HP-20, Toyopearl HW-40, Sephadex LH-20, MCI Gel CHP-20, silica gel column chromatography, and preparative HPLC, and their structures were elucidated on the basis of spectral data and physiochemical properties. RESULTS Twenty compounds were elucidated as vanillic acid(1), ferulic acid(2), 4-hydroxyacetophenone(3), dihydroconiferylalcohol(4), loliolide(5), 4-hydroxy-3-methoxyphenylprop-8-ene 4-O-??-D-xylopyraosyl-(1??6)-??-D-glucopyranoside(6), 1H-indole-3-carbaldehyde(7), 5,7-dihydroxychromone(8), pyromeconic acid(9), erigeside D(10), methyl syringate 4-O-??-D-glucopyranoside(11),(7S,8R)-urolignoside(12), homoeriodictyol(13), pinobaksin(14), chrysin(15), hispidulin(16), chryseriol(17), cyclomorusin(18), cirsimaritin(19), and naringenin(20), respectively. CONCLUSION Compounds 1-8 and 11-19 is isolated from this plant for the first time.     

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??OBJECTIVE To investigate the Polygonum capitatum's influences on the related indicators in db/db mice which is the obesity model of type 2 diabetes mellitus. METHODS Randomly dividing the mice into 5 groups:model group, rosiglitazone hydrochloride group, low-, moderate- and high-dose groups of Polygonum capitatum (5, 10, 20 g??kg^-1), make the db/m mice as blank control. Give the medicine for four weeks. The body weight, blood sugar were determined every week.At the end of fourth week, measuring the glucose tolerance and INS, IL-6 in serum. After all the mice were killed, testing the cholesterol and triglyceride in liver and skeletal muscle and then collecting the liver tissue for HE staining. At the meantime, the expression level of AMPK and GLUT4 in liver were detected by Q-PCR. RESULTS Polygonum capitatum can improve the body weight, blood sugar and glucose tolerance of db/db mice as well as the content of INS and IL-6 in serum, but increase the content of SOD and decrease the content of MDA in mice, furthermore, the cholesterol and triglyceride levels in the liver and skeletal muscle were also declined. HE staining showed that Polygonum capitatum could reduce the number of vacuoles in the liver of db/db mice, and make its shape more complete and ordered. What's more, raising the expression of AMPK and GLUT4 in the liver. CONCLUSION Polygonum capitatum can improve the condition of insulin resistance state, alleviate inflammation and advance the ability of db/db mice, which can also reduce the number of vacuoles in liver, and relieve the tissue lipid metabolic disorder. Meanwhile, Polygonum capitatum can promote the uptake of glucose in liver tissues, which is resulted from up-regulation of expression in hepatic AMPK and GLUT4 gene.     

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??OBJECTIVE To synthesize the impurity A of sitagliptin which is a highly selective DPP-4 inhibitor used for treatment of type 2 diabetes. METHODS 1-{3-Trifluoromethyl-5,6-dihydro-1,2,4-triazo[4,3-a]piperazin-7(8H)-yl}-4-(2,4,5-trifluorophenyl)butane-1,3-dione was prepared from 2,4,5-triflurophenylacetic acid, meldrum's acid and 3-trifluromethyl-5,6,7,8-tetrahydro-1,2,4-triazolo[4,3-a]pyrazine hydrochloride with one-pot reaction, followed by reduction with sodium borohydride to yield the impurity A of sitagliptin. RESULTS The structure of the impurity A of sitagliptin was characterized by IR, MS, and ¹H-NMR. CONCLUSION The established synthetic route of the impurity A in this study has not been reported in the literature, and has the advantages of low-cost, easy operation, mild reaction, and high overall yield.     

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??OBJECTIVE To probe into the operation and management of quality control of chemotherapy in cancer hospital, so as to improve the efficacy and standardization of chemotherapy. METHODS By summarizing management practice of clinical chemotherapy of pharmacist inrapy drugs, and analyzing the pharmacists?? work and problems in cancer hospital, combining with domestic and foreign literature reports of pharmacists in quality control of chemotherapy, the concept and scope of chemothe sting in quality control of chemotherapy were formulated. RESULTS The scope of quality control of chemotherapy should include standardization of all drugs in the process of chemotherapy; pharmacists' work about quality control mainly includes two aspects: the quality control of pharmaceutical affairs management and clinical pharmaceutical care; the barriers of quality control are the lack of clinical knowledge and pharmaceutical guidelines, and the records of patients' chemotherapy.CONCLUSION With the pharmacist participating in clinical chemotherapy, pharmacists have the ability to become the interdisciplinary and multidisciplinary cooperation in tumor chemotherapy of participants, so as to guarantee the specification of the chemotherapy.     

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??Quercetin could affect both the in vivo and in vitro transport of a variety of commonly used drugs by modulating the uptake transporter organic anion transporter polypeptides (OATPs), organic anion transporters (OATs), efflux transporter P-glycoprotein (P-gp), multidrug resistance-related protein (MRP) and breast cancer resistance protein (BCRP), respectively. Quercetin can regulate various drug transporters, thereby affecting other drugs in vivo process.     

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??OBJECTIVE To investigate the contents of oligosaccharides in 37 batches of Morinda officinalis How samples from different habitats and germplasm resources at various ages. METHODS HPLC-ELSD method was used to determine the contents of four oligosaccharides, i.e sucrose, 1-kestose, nystose and 1^F-fructofuranosylnystose in Morinda officinalis How at different ages from different habitats and germplasm resources. The relationships among the several factors were analyzed. RESULTS The samples from Guangdong Province had larger amounts of sucrose, 1-kestose and 1^F-fructofuranosylnystose than those from Fujian, Guangxi and Hainan Provinces. The content of nystose in the samples from Guangdong Province was similar with those from Fujian Province. The contents of sucrose and 1-kestose were the highest in the samples of 2.5 years old, while the contents of nystose and 1^F-fructofuranosylnystose were the highest in the samples of 4 years old. The germplasm resources of small leaf had higher content of oligosaccharides than the large leaf germplasm in Guangdong Province, and different germplasm resources of Morinda officinalis How also had different morphological characteristics. CONCLUSION The contents of four Morinda officinalis How oligosaccharides vary with habitat, germplasm and age. This research may provide references for the quality control of Morinda officinalis How.     

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??OBJECTIVE To identify Dalbergiae Odoriferae Lignum and its adulterants using DNA barcoding. METHODS ITS2 is one of the popular DNA barcoding in the identification of traditional Chinese medicine. In this paper,the ITS2 regions of Dalbergiae Odoriferae Lignum and its adulterants were amplified and sequenced bi-directional.The length and GC content of ITS2 sequence were analyzed through MEGA5.0 software. The genetic distances were computed by kimura 2-parameter (K2P) model. Dalbergiae Odoriferae Lignum and its adulterants have been identified through the species identification system for traditional Chinese medicine and neighbor-joining (NJ) phylogenetic tree. RESULTS The sequence lengths of ITS2 of Dalbergiae Odoriferae Lignum were 216 bp, and the GC content was 68.5%. The minimum K2P interspecific genetic distances of Dalbergiae Odoriferae Lignum and its adulterants were 0.009, which was larger than that of the intraspecific genetic distances of Dalbergiae Odoriferae Lignum.The Dalbergiae Odoriferae Lignum and its adulterants can be obviously identified using the Species identification System and NJ phylogenetic trees.CONCLUSION ITS2 Regions as DNA barcode can identify Dalbergiae Odoriferae Lignum and its adulterants accurately.     

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??Topical ocular medication is commonly used for eye diseases treatment.In view of low bioavailability and poor efficacy of traditional ocular preparations,the development of novel ocular drug delivery systems has become a great challenge in pharmaceutics.In recent years, nano preparations have been widely used for ocular drug delivery systems. At present, several nanocarriers, such as polymeric micelles, nanoparticles, nanosuspension, liposomes, emulsion, and dendritic polymers have been developed for ocular drug delivery.There are some other new dosage forms, such as in-situ gelling systems, implants, contact lenses, and microneedles are also under continuous research. The aim of development of these new dosage forms is to improve the drugs' ocular bioavailability and therapeutic effects.In this paper,the development in these areas in recent years are reviewed in order to provide reference for the development of new ocular drug delivery systems.     

碱蓬与盐地碱蓬红外光谱的三级鉴定

目的:对碱蓬和盐地碱蓬进行红外光谱鉴定。方法:采用红外光谱三级鉴定法。结果:二者的一维谱图比较相似,但一些吸收峰的峰形、峰位和峰强具有一定的差异,碱蓬1646 cm-1处的相对峰强度高于1061 cm-1处的吸收峰,而盐地碱蓬正好相反;二阶导数谱图在1500 cm-1¹300 cm-1、1110 cm-11300 cm-1、1110 cm-1⁷00 cm-1区间内部分峰形、峰强和二维相关谱中自动峰的峰数均有明显区别。结论:红外光谱三级鉴定法可以快速、准确地鉴别碱蓬和盐地碱蓬。     

基于灰色关联度的旋覆花黄酮类有机成分与无机成分分析

目的:在建立不同产地旋覆花黄酮类有机成分指纹谱和无机成分轮廓谱的基础上,探讨有机成分与无机成分的相关性,为全面控制旋覆花药材的质量提供前期基础。方法:采用高效液相色谱法(HPLC)建立有机成分指纹谱,采用电感耦合等离子体质谱法(ICP-MS)建立无机元素轮廓谱,并通过灰色关联度法探讨两者的相关性。结果:从有机成分指纹图谱中获得18个共有指纹峰;从无机元素轮廓谱中获得13种共有特征元素;灰色相关分析结果显示1号色谱峰与K,Ca相关性最强,2号,17号色谱峰与Na,Mg,Mn相关性最强,4号,13号色谱峰与Zn相关性最强,5号色谱峰与Fe相关性最强,9号,11号色谱峰与Al相关性最强,相关系数均0.969 0。结论:该研究在控制旋覆花黄酮类有机成分和无机元素含量基础上进行关联分析,二者存在较强相关性,说明控制有机成分含量的同时也可以部分反应无机元素含量高低,为建立一种全面的质量控制方法及系统评价旋覆花药材质量提供实验参考。     

煅硼砂X射线衍射指纹图谱研究

目的:建立中药煅硼砂X射线衍射指纹图谱,为煅硼砂质量评价提供新方法。方法:采用X射线衍射技术对煅硼砂样品进行定性分析,并对各样品共有峰进行相似度分析。结果:获得了8个煅硼砂样品的X射线衍射图谱,其中7个样品衍射图谱几何拓扑特征基本一致;利用该7批煅硼砂样品X衍射图谱得到煅硼砂的X射线衍射指纹图谱;并以指纹图谱为对照,根据煅硼砂X射线衍射图谱中各特征峰峰高强度,以夹角余弦法和相关系数法计算各样品X射线衍射图谱的相似度,发现不同样品X射线衍射图谱共有峰相似度均较高,与聚类分析结果一致。结论:X射线衍射指纹图谱分析方法专属性强,准确可靠,可实现对煅硼砂的鉴别和质量评价。     

矿物类中药青礞石的XRD Fourier指纹图谱研究

目的:建立青礞石XRD Fourier指纹图谱评价方法,并比较炮制前后指纹图谱的变化.方法:采用粉末X射线衍射技术对青礞石进行分析,并作模糊聚类法分析和相似度评价.结果:建立了以10个共有峰为特征指纹信息的14批青礞石的XRD Fourier指纹图谱分析方法;所分析样品XRD Fourier指纹图谱的10个特征峰晶格间距d(A)及峰位20的均数相关系数、中位数相关系数、均数相似度(夹角余弦值)、中位数相似度(夹角余弦值)均在0.999 9以上.相对强度值Ⅰ/Ⅰo(％)的相关系数均大于0.95,均数相似度(夹角余弦值)、中位数相似度(夹角余弦值)均大于0.97;少数样品XRD Fourier图谱的峰数目和峰强有一定差异;生品与煅制品的XRD Fourier图谱有明显差异.结论:XRD Fourier指纹谱分析法可用于青礞石药材的鉴定与分析.     

二妙丸类方抗湿热证痛风有效部位群指纹图谱比较研究

目的：为探索类方方剂配伍物质基础变化特征，研究二妙丸类方(二妙丸、三妙丸、四妙丸及加味四妙丸)配伍物质基础的关联。方法：建立加味四妙丸抗湿热证痛风有效部位群HPLC指纹图谱，利用对照品确定指纹图谱共有峰成分、组方药有效部位色谱峰归属以及有效部位群共有峰的组方药有效部位来源，测定二妙丸类方抗湿热证痛风有效部位群指纹图谱，比较指纹图谱共有峰成分特征及配伍变化。结果：加味四妙丸有效部位群有60个共有峰，分别来源于组方药生物碱、黄酮、有机酸部位。基础方与类方间有效部位群指纹图谱共有峰在数目及相对峰面积比值方面呈现一定的变化规律。结论：二妙丸及其类方有共同的物质基础，从基础方到各类方，抗湿热证痛风物质基础的配伍变化具有相关性。     

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??OBJECTIVE To discuss the problem of instrumental test method of clarity and degree of opalescence of liquids in the general notice 0902 of China Pharmacopeia(Ch.P)2015, find out the causes and offer solutions. METHODS The test methods of clarity in Ch.P 2015 and European Pharmacopeia (EP) 8.0 were compared, including instrumental types, applicability, sample requirements, and result evaluation. RESULTS The primary opalescent suspension for the instrumental method is the same as the visual method, using the absorbance (A=0.12-0.15) at 550 nm to control the opalescence. Because the resolving power of the instrumental method is far higher than the visual method, the limit becomes interval distribution instead of simple point. The opalescent value (NTU) of the upper limit (A=0.15) is about 1.35 times of the lower limit (A=0.12).When the NTU value of the test liquid is in this interval, the result evaluation will be hard.CONCLUSION The preparation of the primary opalescent suspension in Ch.P 2015 is different from EP8.0. For this reason, the limit set by Ch.P 2015 is actually stricter than that of EP8.0. The opalescent value of the standard solution used by Ch.P 2015 is about 75% of that used by EP8.0.     

青藤碱-β-环糊精包合物的制备及表征

目的研究青藤碱-β-环糊精包合物的制备与性质。方法通过溶液共混法制备青藤碱-β-环糊精包合物,纯化后利用体式显微镜观察各包合物的结晶形态,并通过红外光谱(IR)、差热分析(DSC)、X射线粉末衍射(XRD)、核磁共振氢谱(1H-NMR)等方法对包合物进行表征。结果对青藤碱-β-CD包合物,XRD检测到一组新的特征衍射峰,2θ分别为6.98°、8.48°、9.74°、9.92°、18.50°;DSC能观察到包合物与物理混合物存在明显不同;IR检测到青藤碱的部分特征吸收峰,受包合物形成的影响其强度降低,峰形变宽,发生位移或消失等现象;1H-NMR能检测到β-CD空腔内壁的两个质子H-3和H-5受包合物形成的影响其化学位移减小。这些表征试验均证实,青藤碱-β-环糊精包合物已经形成。结论青藤碱与β-环糊精可形成稳定的包合物;β-环糊精可显著增加青藤碱的溶解度。     

基于特征图谱的金银花与山银花(灰毡毛忍冬)质量表征比较研究

目的阐明金银花与山银花药学质量表征的共性与特性。方法采用HPLC-DAD法,Waters XBridge C18分析柱(250 mm×4.6 mm,5μm),以乙腈-0.4%磷酸水溶液为流动相梯度洗脱,流速1.0 mL/min,检测波长为211 nm,柱温30℃,建立金银花和山银花特征图谱质量表征方法;基于特征图谱中的特征峰的所属化学类型及代表性成分的峰面积和含量对15批金银花和10批山银花饮片进行药学质量表征,并对二者的药学质量特点进行比较分析。结果(1)建立的金银花和山银花的特征图谱及质量表征方法表征了二者质量表征特征值:特征峰、相对保留时间、相对峰面积、代表性成分含量及其相对含量。(2)金银花和山银花均具有特征峰30个,其药学架构涵盖4种化学类型,其中金银花/山银花各类型特征峰数目分别为:环烯醚萜类16/6,酚酸类8/11,黄酮类4/5,三萜皂苷类2/8个。(3)二者具有共有特征峰15个,其中环烯醚萜类6个、酚酸类6个、黄酮类2个、三萜皂苷类1个。(4)在金银花/山银花特征峰中指认了11个代表性成分:环烯醚萜类3/2、酚酸类6/6、黄酮类1/1、三萜皂苷类1/2;其代表性成分含量(mg/g)分别为:断氧化马钱子苷(21.756~29.826)/(6.936~14.643)、獐芽菜苦苷(12.204~30.139)/(26.109~31.608)、当药苷(13.806~23.27/(-),绿原酸(24.686~36.595)/(36.796~42.979)、异绿原酸A(14.010~20.452)/(50.544~58.013)、异绿原酸C(2.896~4.681)/(6.986~7.960)、异绿原酸B(0.935~1.260)/(1.389~1.738)、新绿原酸(0.888~1.560)/(2.025~2.635)、隐绿原酸(0.565~0.852)/(0.947~1.122),木犀草苷(0.579~0.690)/(0.527~0.642),灰毡毛忍冬皂苷乙(14.471~20.243)/(35.487~54.576)、川续断皂苷乙(-)/(31.191~35.731)。结论建立的特征图谱质量表征方法可准确地表征金银花与山银花的药学质量,二者质量表征共性为:具有相同的药学架构及部分共有特征成分;又具有明显的特性:金银花环烯醚萜类特征峰较多,当药苷为其特有环烯醚萜类成分,断氧化马钱子苷和木犀草苷的含量高于山银花;而山银花酚酸类和三萜皂苷类特征峰较多,川续断皂苷乙为其特有三萜皂苷类成分,异绿原酸A、灰毡毛忍冬皂苷乙、绿原酸、獐芽菜苦苷、异绿原酸C、新绿原酸、异绿原酸B和隐绿原酸的含量均高于金银花。研究结果可为金银花与山银花的质量控制及合理应用提供科学依据。     

首批肝素相对分子质量国家对照品的建立

目的《中国药典》2015年版二部肝素钠、肝素钙新增相对分子质量与相对分子质量检查项,需建立首批肝素相对分子质量国家对照品及系统适用性对照品。方法以《美国药典》肝素相对分子质量测定用对照品(USP heparin sodium molecular weight calibrant,批号:F0L483)为肝素相对分子质量对照品,以《美国药典》肝素相对分子质量系统适用性对照品(USP heparin sodium identification,批号:G1L413)为肝素相对分子质量系统适用性对照品,采用《中国药典》2015年版二部肝素钠“相对分子质量与相对分子质量分布”检查法,对肝素相对分子质量国家对照品待标品(批号:140819-201501)及肝素国家对照品待标品(批号:140818-201501)进行相对分子质量与相对分子质量分布测定,由全国12个药检所及肝素生产厂家实验室协作标定。结果对肝素相对分子质量国家对照品待标品(批号:140819-201501)相对分子质量5000~42000的20个点的百分面积进行标定,对实验室内误差进行考察,12个实验室中有2个实验室(2号、7号)部分点的标准差(standard deviation,SD)为1%~2%,其余10个实验室的SD值均小于1%,对实验室间误差进行考察,20个数据点的SD值均小于1%。相对标准偏差(relative standard deviation,RSD)均小于10%。肝素国家对照品待标品重均相对分子质量实验室内SD值除2号实验室外,其余实验室SD小于180,实验室间SD为180,实验室间RSD为1.1%。结论经国家药品标准物质委员会审定后批准,肝素相对分子质量国家对照品待标品(批号:140819-201501),附带宽分布标样表,及肝素国家对照品待标品(批号:140818-201501),重均相对分子质量16200,可以用于《中国药典》2015年版二部肝素钠、肝素钙相对分子质量与相对分子质量分布检查使用。     

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??OBJECTIVE To clarify the crystal forms of the active pharmaceutical ingredient and preparations of felodipine from different sources, and explore the relationship between quality and efficacy of felodipine and its crystal form. METHODS Crystal form characterization of the active pharmaceutical ingredient from different sources was carried out by powder X-ray diffraction (PXRD), infrared spectroscopy (IR) and differential scanning calorimetry (DSC). The Origin software was used to analyze the crystal forms of felodipine in the sample preparations from different sources. Biological evaluation in vivo was conducted by using whole animals. RESULTS There were some differences in the crystal state of the active pharmaceutical ingredient from different sources, but the main components were basically the same, all of which were type I. Biological studies showed significant differences in the main pharmacokinetic parameters of felodipine sustained release tablets from different sources. Among them, the ??_max, t_max, t_1/2, and AUC_0-t had maximal 1.8, 1.4, 8.2 and 1.5 times of differences. CONCLUSION Although the main crystal forms of felodipine bulk drug from different origins are consistent, the crystal state significantly changes after the preparation process. This finding is of important scientific significance to guide the improvement of process and product quality.