高效液相色谱-电喷雾-质谱法分析山茱萸中的化学成分

目的 建立山茱萸中化学成分的高效液相色谱-电喷雾-质谱分析方法.方法 采用Zorbax SB-C18色谱柱,乙腈-水二元梯度洗脱;Agilent电喷雾离子阱多级质谱仪;负离子检出模式.结果 在负离子检出模式下,山茱萸的总离子流色谱图特征性很强,通过质谱中的主要碎片对莫罗忍冬苷、山茱萸裂苷、没食子酸、1,2,3-三-O-没食子酰葡萄糖和1,2,3,6-四-O-没食子酰葡萄糖5种主要成分进行了结构解析.结论 在谱负离子检出模式下,多数化学成分响应较好,为山茱萸药材质量控制提供了一种新的方法.     

LCMS-IT-TOF法快速分析薄荷黄酮部位的主要化学成分

目的快速分析鉴别薄荷黄酮部位的化学成分。方法采用高效液相色谱-离子阱-飞行时间质谱法(LCMS-IT-TOF)对薄荷黄酮部位化学成分进行分析,Sunfire C18色谱柱(4.6 mm×150mm,5μm),甲醇(A)-水(B)为流动相进行梯度洗脱,电喷雾离子源为质谱离子源,同时采用正、负离子检测模式,获得不同化合物的多级质谱数据。结果根据高分辨质谱结果和MS/MS碎片信息,结合对照品质谱信息及相关文献,共鉴定推断出12个黄酮类化合物,其中4个黄酮苷:芹菜素-7-O-芸香糖、香叶木苷、木犀草素-7-O-芸香糖、蒙花苷;6个黄酮苷元:5,6-二羟基-7,8,3',4'-四甲氧基黄酮、栀子黄素B、5,6-二羟基-7,8,4'-三甲氧基黄酮、刺槐素、5-羟基-6,7,8,3',4'-五甲氧基黄酮、香叶木素;1个黄酮醇苷:芦丁;1个二氢黄酮苷:橙皮苷。结论 LCMS-IT-TOF能快速有效地分析薄荷黄酮部位的化学成分,为其进一步研究提供物质基础。     

基于UHPLC-Q-Orbitrap HRMS快速鉴定桂枝中水溶性成分

目的:应用超高效液相色谱-四级杆/静电场轨道肼高分辨质谱联用(UHPLC-Q-Orbitrap HRMS)技术,快速识别与鉴定桂枝中水溶性化学成分。方法:采用Waters Acquity UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),以0.1%甲酸水溶液-乙腈为流动相,梯度洗脱。质谱采用ESI源,四级杆/静电场轨道肼质量分析器,正负离子切换扫描采集数据。根据高分辨质谱给出的精确分子量和二级碎片离子等信息,并结合对照品和相关文献对桂枝水提液中的化学成分进行指认。结果:共鉴定桂枝水提液中20个化合物,涵盖苯丙素、苯丙素苷、黄酮、木脂素、倍半萜和小分子酚酸等多种类型的化合物。结论:建立的UHPLC-Q-Orbitrap HRMS方法可快速鉴定桂枝中的化学成分,为深入探讨其药效物质基础、质量控制以及方剂配伍等提供了科学的依据。     

茯苓95％乙醇提取物三萜类化学成分的UPLC-IT-TOF/MS分析

目的 采用超高效液相色谱串联离子阱飞行时间质谱(UPLC-IT-TOF/MS)技术定性分析茯苓95％乙醇提取物的三萜类化学成分.方法 采用UHPLC XB-C18色谱柱,甲酸/水(0.05/100,v/v)-乙腈作为流动相,梯度洗脱,流速为0.20 mL/min;紫外检测波长范围为190～400 nm.使用ESI离子源,三氟乙酸钠校正,电喷雾正负离子同时检测,Shimadzu Composition Formula Predictor软件定性分析茯苓三萜类化合物.结果 通过多级质谱数据分析,结合氮规则和Scifinder数据库检索,从茯苓醇提取物中鉴定了22个三萜类成分,结构类型包括羊毛甾-8-烯型三萜、羊毛甾-7,9(11)-二烯型三萜和其他羊毛甾三萜类型.结论 通过LC-MS快速分析了茯苓醇提取物中三萜类成分,为其药效物质基础和质量控制提供了依据.     

茯苓95％乙醇提取物三萜类化学成分的UPLC-IT-TOF/MS分析

目的 采用超高效液相色谱串联离子阱飞行时间质谱(UPLC-IT-TOF/MS)技术定性分析茯苓95％乙醇提取物的三萜类化学成分.方法 采用UHPLC XB-C18色谱柱,甲酸/水(0.05/100,v/v)-乙腈作为流动相,梯度洗脱,流速为0.20 mL/min;紫外检测波长范围为190～400 nm.使用ESI离子源,三氟乙酸钠校正,电喷雾正负离子同时检测,Shimadzu Composition Formula Predictor软件定性分析茯苓三萜类化合物.结果 通过多级质谱数据分析,结合氮规则和Scifinder数据库检索,从茯苓醇提取物中鉴定了22个三萜类成分,结构类型包括羊毛甾-8-烯型三萜、羊毛甾-7,9(11)-二烯型三萜和其他羊毛甾三萜类型.结论 通过LC-MS快速分析了茯苓醇提取物中三萜类成分,为其药效物质基础和质量控制提供了依据.     

基于HPLC-Q-TOF-MS/MS的广枣果肉化学成分分析

目的 采用高效液相色谱-四级杆-飞行时间串联质谱(HPLC-Q-TOF-MS/MS)法对广枣醇提物的主要化学成分进行分析鉴定.方法 采用回流提取法制备广枣醇提物,以Agilent TC-C18(4.6mm×250 mm,5μm)柱为分析柱,并以0.2％甲酸-甲醇溶液为流动相,流速0.7 mL/min,柱温30℃,进样量25 μL,进行梯度洗脱;质谱采用电喷雾离子源,毛细管电压4.0 kV,干燥器流速10.0 L/min,干燥器温度350℃,雾化器压力35.0 psi(1 psi=6 894.8 Pa),正负离子模式下扫描采集数据,并对各主要色谱峰进行归属.结果 通过正负离子质谱信息及元素组成分析,并结合相关文献和对照品数据对照,共鉴定出42种化合物,主要为氨基酸类、有机酸类及黄酮类,其中首次在广枣中发现的成分有17种.结论 HPLC-Q-TOF-MS/MS兼具色谱的高分离特性和质谱的高灵敏度双重优势,能对广枣的主要化学成分进行定性分析,可为广枣药效物质的基础研究提供依据.     

UPLC/ESI-Q-TOF MS法分析远志中的化学成分

[目的]阐明远志中的化学成分。[方法]采用超高效液相色谱-电喷雾离子化-四级杆飞行时间串联质谱（UPLC/ESI-Q-TOF MS）法分析远志中的化学成分,采用Masslynx V 4.1软件,通过分析准分子离子和二级碎片离子信息,并进一步根据标准品的色谱保留时间和质谱裂解规律,鉴定远志中的化学成分。[结果]鉴定了远志中29个化学成分,主要为口山酮、低聚糖酯、皂苷类成分。[结论]总结归纳了远志药材中主要化学成分的质谱裂解规律,阐明了远志中的主要化学成分。     

UPLC-Q-Exactive四极杆-静电场轨道阱高分辨质谱联用分析黄芪根及其茎叶中黄酮和皂苷类成分

目的利用UPLC-Q-Exactive四极杆-静电场轨道阱高分辨质谱仪联用技术,分析黄芪根及其茎叶中的黄酮和皂苷类成分。方法以90%甲醇提取黄芪根及其茎叶作为提取液制备供试品溶液,采用Hypersil GOLD C18(100×2.1 mm,1.9μm)进行色谱分离,以乙腈-0.1%甲酸溶液为流动相进行梯度洗脱,质谱采用正负离子监测模式、全扫描及自动触发二级质谱扫描的方法,对黄芪根及其茎叶中的黄酮和皂苷类成分进行分析和鉴定。结果通过高分辨质谱采集的数据,最终黄芪根中共鉴定了18种化合物,黄芪茎叶中共鉴定了17种化合物。其中,黄芪根中有12个化合物通过与对照品进行比对明确指认,黄芪茎叶中有10个化合物通过与对照品进行比对明确指认。结论通过利用UPLC-Q-Exactive四级杆-静电场轨道阱高分辨质谱技术,将黄芪根及其茎叶中黄酮和皂苷类成分进行了指认和比较,两者有12个共有成分、11个区别成分,表明黄芪根与其茎叶相比较,虽来源于药用植物黄芪的不同药用部位,但就其主要化学成分而言,有很多相同的成分,也有区别的成分,相关这些区别成分的研究为进一步探究黄芪茎叶药效物质基础指明了方向。     

四妙勇安汤水提物大鼠吸收入血成分研究

目的通过对四妙勇安汤水提物入血成分的研究,初步阐明该复方的药效物质基础。方法采用高效液相色谱-离子阱-飞行时间质谱(LCMS-IT-TOF)联用技术,在电喷雾离子源的正、负离子模式下,对四妙勇安汤水提物、大鼠灌胃给药后的血清和空白血清进行检测。以甲醇对血清样本进行前处理,采用Inertsil ODS-3色谱柱,以乙腈(A)-水(含0.1%甲酸)(B)为流动相进行梯度洗脱,根据化合物的多级质谱碎片,结合参考文献和对照品初步确定四妙勇安汤水提物入血成分。结果四妙勇安汤灌胃给药后在大鼠血清中发现14个入血成分,其中10个来自该复方的原型成分,其余4个可能为代谢产物。9个色谱峰被确认为哈巴苷、绿原酸、马钱苷、当药苷、甘草苷、金丝桃苷、安格洛苷C、异绿原酸C和哈巴俄苷。结论四妙勇安汤入血成分是各组方药味配伍后共同作用的结果,本研究可为四妙勇安汤的药效物质基础和进一步的体内代谢研究提供参考。     

山莨菪碱及其大鼠肠内菌体外代谢物的液相色谱-质谱法分析

目的 用液相色谱-电喷雾离子阱串联质谱联用法研究山莨菪碱在大鼠肠内菌中的代谢。方法 以山莨菪碱优化色谱及质谱条件，总结其色谱及质谱行为规律。将山莨菪碱与大鼠肠内菌体外厌氧温孵培养，并与空白样品及山莨菪碱对照品进行比较，依据被测物的多级质谱数据，鉴定代谢物并阐述其结构。结果 在温孵液中发现了山莨菪碱的脱水及水解代谢产物，即脱水山莨菪碱、6β-羟基托品和托品酸。结论 该方法灵敏、快速、简单，适合于药物代谢分析。     

Acupuncture Treatment of Vomiting

CASE HISTORY A female patient, 46 years old, head of the foreign affairs department of a certain university in Beijing, paid her first visit on October 9, 2006, with the chief complaint of vomiting for one month. She got vomiting after meals in early September. Before that, she had discomfortable sensation in the stomach due to angry with others, but she didn't pay much attention. Later, it developed into vomiting after eating. After the vomiting, the discomfort would be relieved, but with slight hypodynamia. She was once diagnosed as having 'neurogenic vomiting'. Having taken some western and Chinese drugs, the above symptoms were a little bit improved, but she would have nausea upon eating and with regurgitation. Because of the fear for vomiting, she did not dare to have food intake, with body weight reduction of 6 kilos in one month.     

Qiu Baoguo''''s Experience in Treating Consumptive Syndromes after Radio-Chemotherapies

Radiotherapy and chemotherapy are the important modern medical therapies for malignant tumors,yet they can also bring about serious local and systemic toxic side reactions so to decrease the patient;'s life quality,manifested by a series of consumptive symptoms.Having engaged in the combined work of Chinese and western medicine for nearly 50 years,the research fellow Qiu Baoguo in Henan Provincial Academy of TCM has developed his unique views on the TCM study of consumptive syndromes.The author of this essay had once the fortune tO follow Dr.Qiu in clinic,and specially would like to introduce in the following Dr.Qiu's experience in treating consumptive syndromes after radio-chemotherapies for patients with malignant tumor.     

Insomnia Due to Deficiency of Both the Heart and Spleen Treated by Acupuncture-Moxibustion and Chinese Tuina

OBJECTIVE: To observe therapeutic effects of the comprehensive therapy of acupuncture-moxibustion and Chinese Tuina for treatment of insomnia due to deficiency of both the heart and spleen. METHODS: 92 cases were divided randomly into the treatment group (treated by acupuncture-moxibustion and Chinese Tuina) and the control group (treated by acupuncture-moxibustion). RESULTS: The therapeutic effect of the treatment group was obviously superior to that of the control group (the CHI2 test showed P < 0.01). CONCLUSIONS: The comprehensive therapy of acupuncture-moxibustion and Chinese Tuina can give marked therapeutic effects for treatment of insomnia due to deficiency of both the heart and spleen.     

Analysis of CK-19,PDX-1,Nestin,Ngn3 in different donor islet purity in rats

Objective: To investigate if there are the CK-19, PDX-1, Nestin, Ngn3 positive cells in the donor islets of different purity in rats. Methods: Thirty male adult SD rats were randomly divided into 3 groups. Islets were isolated using digestion by ductal injection of collagenase. Group Ⅰ (n=10): Separating cell preparations were not purified, Group Ⅱ(n=10): Islet sediment was purified with 25% Ficoll400 ,Group Ⅲ (n=10): Islet sediment was purified with 25% and 11% Ficoll-400. The levels of protein of CK-19, PDX-1, Nestin and Ngn3 were detected by immunohistochemistry and the mRNA of CK-19, PDX-1, Nestin, Ngn3 was amplified by RT-PCR. Results: After two different purification methods applied, three islet preparations of different purities were obtained. The difference of islet purity was significant among various groups (P＜0.05). Compared with group Ⅱ and group Ⅲ,the protein and mRNA of CK-19, PDX-1, Nestin,Ngn3 were both higher in group Ⅰ; group Ⅲ was poorly expressed. Conclusions: The three different islet purity donor islet have different CK-19, PDX-1, Nestin, Ngn3 positive cells within them, indicating that there are some islet stem cells in the purified donor islet.     

A preliminary screening study on the associated proteins in human psoriasis vulgaris by serum proteomics technologies

Objective：To investigate the optimum screening conditions of associated proteins in human psoriasis vulgaris by serum proteomics technique, and to screen the different expression proteins related with psoriasis vulgaris. Methods：Serum samples of peripheral blood were collected from newly diagnosed psoriasis vulgaris patients in the clinic, and 20 matched healthy persons. Serum albumin IgG was removed by filtering with ProteoExtract Albumin/IgG. After comparative proteomics analysis the different protein spots were identified using 2-DE and MS. Results ：Electrophoresis figures with high resolution and reproducibility were obtained. Three different expression proteins were found only in the serum from psoriasis vulgaris patients, while nine other different proteins expressing from healthy volunteers. Conclusion：The protein expression was different in the serum between the psoriasis vulgaris patients and healthy volunteers. It was hoped that we could find the biomarkers related to psoriasis vulgaris by using proteomics.     

A CASE OF HUGE GASTRIC DISOPYROBEZOAR

PYTOBEZOARS are common bezoars in gastrontestinal tract, commonly seen in stomach and mall intestine,1but huge disopyrobezoars are     

Acupuncture Treatment of Chest Bi Syndrome

CASE HISTORY A male,a retired officer of 61 years old,paid his first visit on May 12,2006.The patient stated that 2 weeks before he suddenly got paroxysmal precordial choking pain,with irregular attacks.Each attack would last several seconds to several minutes.The attack was accompanied with heavy oppressed sensation in the precordial region,palpitation,lassitude,and in severe cases,sweating,which was once diagnosed by a hospital as'coronary heart disease'.Recalling the case history,the patient said that several days before he got angry with others because of some affairs in work,and he was not so used to the life pattern since he had just retired from his busy working post.At usual times,he was quick tempered and peevish.In recent days,he had poor appetite,and loose stool.     

Instructions to Contributors

The English edition of Chinese Journal of Integrative Medicine is edited and published by the Chinese Journal of Integrated Traditional and Western Medicine Press.Original scientific papers of advanced clinical and experimental medicine in the field of complementary/alternative medicine or integrative medicine are expected.     

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