Primary Exploration on Quality Evaluation of Holothurian Sold on the Market by HPLC Fingerprint

以10批不同产地刺参HPlC指纹图谱中的6个共有峰为评价指标,结合相似度分析,对不同刺参质量进行评价和检验。结果表明:不同批次刺参样品的6个色谱峰在指纹图谱分析过程中色谱行为相同,峰面积大,特征性强,能反映刺参的固有化学特征。结合相似度分析,可用于刺参质量评价。An optimized high performance liquid chromatography (HPLC) method was developed for the analysis of holothurian and the HPLC fingerprint was established from 10 batches of the holothurians from different habitats.The HPLC fingerprint showing 6 common characteristic peaks was used to explore the quality evaluation of holothurian and distinguish from the fakes with the similarity analysis.This method is accurate and reliable,providing a scientific basis for the quality control of holothurian and can be used to evaluate the quality of holothurian sold on the market.我国近海海洋综合调查与评价908专项(908-02-05-04):海洋药用生物资源评价和《中华海洋本草》编纂;海洋一所基本科研业务专项(GY-022008T32):海洋绿藻活性成分分析、鉴

Determination of five poisonous elements in holothurian sold on the market by Microwave Digestion with ICP—MS

建立了微波消解—电感耦合等离子体质谱法测定海参中Cu,AS,Cd,Hg,Pb 5种有毒元素含量的方法,采用In元素为内标,利用其回收率对以上5种元素的测定结果进行校正,该方法变异系数(CV%)为0.2%--4.0%,In元素加标回收率为96.7%--104.5%,说明该方法灵敏度高,结果准确可信。利用该方法对10批不同市售海参中5种有毒元素含量进行了测定,结果表明10批市售海参中的AS含量均超标,部分批次海参中的Cd、Pb超标,说明市售海参确实存在有毒元素超标的问题。A method based on microwave sample digestion and inductively coupled plasma-mass spectrometry(ICP—MS) detection was established for determination of Cu,As,Cd,Hg and Pb in holothurian sold on the market.Indium was used as internal standard element to calibrate the results of determination of these five elements.Determination limits of these five elements were in the range of 0.006～0.063 μg/g,coefficient of variation(CV%)were in the range of 0.2%～4.0%,and the recovery of In was in the range of 96.7%～104.5%.The method has been applied to determine the five poisonous elements in ten holothurian samples sold on the market.The results indicated that the over-standard problem of poisonous elements in holothurian sold on the market existed.The content of total arsenic was over standard in all the ten samples,but the over standard problem of lead and cadmium was only found in part of the samples.国家自然科学基金(20675021);中国近海海洋综合调查与评价908专项(908-02-05-04)资

Determination of Theanine in Tea by High Performance Liquid Chromatography-Atmospheric Pressure Chemical Ionization Mass Spectrometry

采用高效液相色谱-大气压化学电离质谱(HPlC-APCI-MS)联用技术,建立了茶叶中茶氨酸的含量测定方法。实验采用C8柱,以甲醇-水为流动相,等度洗脱,采用正离子大气压化学电离质谱(SIM模式)进行测定,可以获得稳定的质谱信号,并采用正交实验设计对APCI-MS仪器条件进行了优化。结果表明,本文建立的HPlC-APCI-MS方法操作简便、重现性好,灵敏度较紫外检测器有很大的提高,可用于微量茶氨酸的快速测定。HPLC coupled online with atmospheric pressure chemical ionization MS technique was developed for the qualitative and quantitative determination of theanine in tea.The theanine and other compounds in the tea extract were separated on an Alltima C8 column with methanol and water (10:90 v/v) as mobile phase, with flow rate of 0.6 ml/min and APCI-MS SIM m/z 175.1 detection.In the positive APCI mode, sensitive and stable MS signal could be obtained by APCI-MS (SIM m/z 175.1) detection, and the APCI-MS conditions were also optimized by orthogonal design.The results indicated that HPLC-APCI-MS method was simple, sensitive and reliable for the determination of theanine in tea.It was important that the detection sensitivity was improved greatly by APCI-MS than UV.Eight tea samples from Fujian province were analysed using the established methods.福建省科技厅茶叶指纹图谱质量控制研究项目(2006N0043);海洋一所基本科研业务专项(GY-022008T32)资

Study on HPLC Fingerprint of Chinese Marine Medicine Dried Scallop

目的建立海洋中药干贝高效液相色谱(HPlC)指纹图谱分析方法 ,为其质量控制和药材鉴别提供依据。方法采用反相AllTIMA-C18柱,水(A)和乙腈(b)为流动相,梯度洗脱,流速为0.8Ml/MIn,检测波长210nM,柱温20℃,进样体积30μl;采用高效液相色谱二极管阵列检测器-质谱联用技术(HPlC-dAd-MS)对其特征峰进行快速分析;采用相似度计算软件用于10批干贝药材的相似度评价。结果初步建立了干贝药材的HPlC指纹图谱,10批干贝药材指纹图谱有9个共有峰,相似度均在0.85以上;HPlC-dAd-MS分析获得的4个特征峰的紫外光谱和质谱信息,可用于干贝药材指纹图谱特征峰以及共有峰的准确确定。结论该方法准确、简单、稳定性好,为干贝药材的真伪鉴别及质量控制提供了科学依据。Objective To establish a chromatographic fingerprint of Dried Scallop,a kind of Chinese marine medicine,by high performance liquid chromatography (HPLC),and apply for quality assessment and control of medicine materials of Dried Scallop.Methods Separation was performed on an Alltima-C18 (250 mm × 4.6 mm,5μm),with mobile phase consisting of water (A) and acetonitrile (B) with gradient elution at the flow rate of 0.8 ml/min.The UV detection wavelength was 210 nm,column temperature was 20℃.Characteristic peaks of the fingerprint could be rapidly analyzed by high performance liquid chromatography-mass spectrometry (HPLC-MS),and the software of similarity analysis was used to calculate the similarity of all the Dried Scallop samples.Results All samples tested contained the same nine peaks,and the similarities of 10 batches of Dried Scallop were more than 0.85.MS and UV spectra of the 4 characteristic peaks obtained using HPLC-MS could be used to accurately confirm the characteristic and common peaks in fingerprint of Dried Scallop.Conclusion This method is simple,accurate and stable,and can provide scientific reference for the identification and quality control of Dried Scallop.国家自然科学基金(No.20602009;20905017);海洋公益性行业科研专项(No.200705011;200805039

Analysis of Alkaloids in Coptis chinensis Franch by High Performance Capillary Electrophoresis-Electrospray Ionization Time of Flight Mass Spectrometry

建立了高效毛细管电泳-电喷雾飞行时间质谱联用(HPCE-ESI-TOF/MS)快速定性分析黄连中生物碱类化合物的分析方法.使用未涂层石英毛细管,以50mmol/L乙酸铵-0.5%甲醇溶液(用氨水调至pH=7.2)作为运行缓冲液,分离电压为25kV;鞘液组成为50%甲醇-49.5%水-0.5%乙酸,鞘液流速为4μL/min;质谱选用正离子模式,碰撞电压(Fragmentor)为100V.结果表明,通过各色谱峰紫外光谱和质谱测得精确分子量结果,结合文献,对黄连中7种生物碱进行了鉴定.表明本方法简便、快速,是黄连中生物碱类化合物快速分离、鉴别的有效方法.A new method for the analysis of alkaloids in Coptis chinensis Franch was established by high performance capillary electrophoresis-electrospray ionization time of flight mass spectrometry (HPCE-ESI-TOF/MS). The real samples were separated by an uncoated capillary. 50 mmol/L ammonium acetate containing 0.5% methanol (pH=7.2) was used as the running buffer, and separation voltage was 25 kV. A coaxial sheath flow interface was used as the CE-MS interface, and a 50% methanol-49.5% water- 0.5% acetic acid mixture was used as the sheath liquid with a flow rate of 4 μL/min. The lens voltages in a positive ion mode with a collision induced dissociation (CID) voltage of 100 V were used for ESI-TOF/MS analysis. Seven alkaloids in Coptis chinensis Franch methanol extracts were separated and identified by CE-DAD and CE-ESI-TOF/MS. The coupling of HPCE separation with accurate mass measurement capability of ESI-TOF/MS provides an attractive tool for the identification of alkaloid compounds in Coptis chinensis Franch.国家自然科学基金重点项目(No.20235020);; 青岛“2004将才计划”(No.04-3-JJ-11);; 共建生物医药研发测试中心(No.LS-05-KJZX-76)资助项目

Identification of Bohai Sea crude oil based on characteristic fingerprinting by MSPD-RP-HPLC

建立渤海原油的高效液相色谱(HPlC)特征指纹图谱,为渤海原油的鉴别提供一种新方法。以氧化铝作为基质固相分散剂进行样品处理,采用HPlC法进行分析,双反相C18色谱柱串联,以乙腈-水为流动相,二元线性梯度洗脱,流速为1.0 Ml/MIn,柱温为20℃,双波长检测226 nM、254 nM,进样量10μl;采用所发展的方法对10批渤海原油样品进行分析,建立渤海原油的HPlC特征指纹图谱,结合相似度分析用于渤海原油的鉴别。该方法具有很好的精密度、重复性和稳定性,10批渤海原油特征指纹图谱有13个共有峰,结合相似度分析可以用于渤海原油样品的鉴别,说明HPlC特征指纹图谱是渤海原油鉴别的有力工具。Based on the high performance liquid chromatography(HPLC) characteristic fingerprinting,a new method for crude oil identification of Bohai Sea was developed.The sample pretreatment was done using matrix solid-phase dispersion,and Al2O3 was used as the dispersant.The chromatographic fingerprints were determined by injecting 10 L sample solution each time on two reverse phase C18 columns in series with the gradient elution solvent system composed of water and acetonitrile.The flow rate was 1.0 mL/min,the column temperature was maintained at 20℃ and the signals were acquired at 226 nm and 254 nm.The characteristic fingerprints of crude oil were established by analysis of ten representative samples derived from Bohai Sea,and identification was carried out by the similarity analysis of the characteristic fingerprints.The method was ideally suited for the fingerprinting of Bohai Sea crude oil with good precision,repeatability and stability.13 peaks were selected as the common peaks of the characteristic fingerprint and used for the similarity analysis,which could be applied to distinguish crude oil of Bohai Sea from that of other sources.The characteristic HPLC fingerprinting technique thus was a powerful tool for the identification of crude oil originated from Bohai Sea.海洋公益性行业科研专项(200705011;201005034-3);中国海监技术支撑体系项目;2008年海洋环境保护及节能减排专

Simultaneous determination of 7 nucleosides in Asterias rollestoni using reversed-phase high performance liquid chromatography

建立了罗氏海盘车中7种核苷化合物的反相高效液相色谱分析测定方法。采用超声波辅助提取,选用两根不同的C18色谱柱串联,以甲醇和0.2%(体积分数)乙酸/水溶液为流动相梯度洗脱分离。优化的色谱条件为:柱温为室温,检测波长为260nM,流速为0.8Ml/MIn,进样量为20μl。结果表明,7种核苷化合物在一定的浓度范围内线性关系良好,次黄嘌呤和胸苷的线性范围为0.65~40Mg/l,尿苷、黄嘌呤和肌苷的线性范围为0.80~40Mg/l,胸腺嘧啶的线性范围为1.15~40Mg/l,鸟苷的线性范围为0.50~40Mg/l。样品中7种核苷化合物的加标回收率为90.00%~105.00%,相对标准偏差为0.72%~3.23%。该方法操作简便、灵敏度高、重复性好,回收率高,适用于罗氏海盘车中7种核苷类成分的同时分析,也可用于罗氏海盘车的质量控制和综合评价。A method for the simultaneous determination of 7 nucleosides in Asterias rollestoni was devel-oped using reversed-phase high performance liquid chromatography ( RP-HPLC) .Analytes were extracted by ultrasonic-assisted extraction and separated on two different C18 columns,which were connected in se-ries,under the gradient elution with the mobile phases of methanol and 0.2% ( v/v) acetic acid/water at room temperature.The chromatographic conditions were as follows: flow rate,0.8 mL/min; detection wavelength,260 nm; injection volume,20 μL.Under the optimized conditions,good linear relationships between the values of mass concentrations and the peak areas of hypoxanthine,uridine,xanthine,thy-mine,inosine,guanosine and thymidine were observed in the ranges of 0.65-40,0.80-40,0.80-40,1.15-40,0.80-40,0.50-40,and 0.65-40 mg/L,respectively.The relative standard devia-tions were around 0.72%-3.23% and the recoveries were around 90.00%-105.00%.The results showed that the developed method is sensitive,accurate and reproducible.It is suitable for the analysis of nucleosides in Asterias rollestoni with high recoveries and it is expected to be used for the quality control and evaluation of Asterias rollestoni.国家自然科学基金项目(20905017);海洋公益性行业科研专项(200705011;200805039);海洋局青年基金项目(2010140);海洋一所基本科研业务专项(GY-022008T32;2010G25);中国科学院实验海洋生物学重点实验室开放基金课

Analysis of alkaloids in Coptis chinensis Franch by high performance capillary electrophoresis-electrospray ionization time of flight mass Spectrometry

A new method for the analysis of alkaloids in Coptis chinensis Franch was established by high performance capillary electrophoresis-electrospray ionization time of flight mass spectrometry (HPCE-ESI-TOF/MS). The real samples were separated by an uncoated capillary. 50 mmol/L ammonium acetate containing 0.5% methanol (pH=7.2) was used as the running buffer, and separation voltage was 25 kV. A coaxial sheath flow interface was used as the CE-MS interface, and a 50% methanol-49.5% water- 0.5% acetic acid mixture was used as the sheath liquid with a flow rate of 4 mu L/min. The lens voltages in a positive ion mode with a collision induced dissociation (CID) voltage of 100 V were used for ESI-TOF/MS analysis. Seven alkaloids in Coptis chinensis Franch methanol extracts were separated and identified by CE-DAD and CE-ESI-TOF/MS. The coupling of HPCE separation with accurate mass measurement capability of ESI-TOF/MS provides an attractive tool for the identification of alkaloid compounds in Coptis chinensis Franch

类泛素蛋白及其中文命名

泛素家族包括泛素及类泛素蛋白,约20种成员蛋白.近年来,泛素家族领域取得了迅猛发展,并已与生物学及医学研究的各个领域相互交叉.泛素家族介导的蛋白质降解和细胞自噬机制的发现分别于2004和2016年获得诺贝尔奖.但是,类泛素蛋白并没有统一规范的中文译名. 2018年4月9日在苏州召开的《泛素家族介导的蛋白质降解和细胞自噬》专著的编委会上,部分作者讨论了类泛素蛋白的中文命名问题,并在随后的\"泛素家族、自噬与疾病\"(Ubiquitinfamily,autophagy anddiseases)苏州会议上提出了类泛素蛋白中文翻译草案,此草案在参加该会议的国内学者及海外华人学者间取得了高度共识.冷泉港亚洲\"泛素家族、自噬与疾病\"苏州会议是由美国冷泉港实验室主办、两年一度、面向全球的英文会议.该会议在海内外华人学者中具有广泛影响,因此,参会华人学者的意见具有一定的代表性.本文介绍了10个类别的类泛素蛋白的中文命名,系统总结了它们的结构特点,并比较了参与各种类泛素化修饰的酶和它们的生物学功能.文章由45名从事该领域研究的专家合作撰写,其中包括中国工程院院士1名,相关学者4名,长江学者3名,国家杰出青年科学基金获得者18名和美国知名高校华人教授4名.他们绝大多数是参加编写即将由科学出版社出版的专著《泛素家族介导的蛋白质降解和细胞自噬》的专家