HPLC及LC-MS测定榛子中氯吡苯脲和多菌灵残留

本文采用高效液相色谱法(HPLC)和液相色谱-质谱法(LC-MS)对干果榛子中氯吡苯脲和多菌灵残留量进行含量测定.HPLC和LC-MS均使用C18色谱柱,含量测定采取等度洗脱,流动相:甲醇-水(55∶45,体积比);体积流量:1.0 mL·min-1;测定波长:260 nm;柱温:30℃.LC-MS采取电喷雾离子源,梯度洗脱,体积流量:0.6 mL·min-1,柱温:30℃.结果表明,榛子中氯吡苯脲与多菌灵存在残留,氯吡苯脲质量浓度在1.00~10.00μg·mL-1范围内线性关系良好,加样回收率在95.58%~100.58%;多菌灵质量浓度在1.005~15.075μg·mL-1范围内具有良好的线性关系,加样回收率在95.61%~104.39%.实验证明,HPLC与LC-MS相结合的方法具有操作简便、灵敏度高、检出限低等优点,能有效地检测到榛子样品中膨大剂氯吡苯脲及杀菌剂多菌灵的残留,并确定其残留量,线性关系和回收率结果均令人满意.根据被检测的8批样品中氯吡苯脲和多菌灵两项农药残留量推断,作为一般干果食用榛子是安全的.

基于系统药理学结合LC-MS/MS技术探讨温性经筋通贴膏治疗类风湿性关节炎的药效物质基础与作用特点

目的通过液相色谱-质谱-质谱联用(LC-MS/MS)技术结合系统药理学研究温性经筋通贴膏治疗类风湿性关节炎的药效物质基础与作用特点。方法通过LC-MS/MS技术结合文献检索获取温性经筋通贴膏活性成分信息,使用Swiss Target Prediction平台进行作用靶点预测;利用GeneCards、DrugBank和OMIM数据库检索与类风湿性关节炎相关的疾病靶点并与活性成分作用靶点进行映射取交集,通过Cytoscape软件构建“活性成分-有效靶点”网络;将共同靶点导入STRING数据库构建蛋白互作网络;应用Metascape数据库进行GO功能及KEGG通路富集分析;采用AutoDock软件进行关键成分与有效靶点的分子对接研究。结果通过应用LC-MS/MS技术从温性经筋通贴膏中共鉴别出142个活性成分,经检索相关文献补充活性成分至174个,与类风湿性关节炎交集靶点175个;预测温性经筋通贴膏可能通过小檗碱、新补骨脂异黄酮、盐酸巴马汀等主要成分,作用于TNF、IL6、AKT1等关键靶点,调控PI3K/Akt1、JAK/STAT、MAPK等信号通路发挥免疫调节与抗炎镇痛作用;在1152组分子对接验证中,结合能小于-5.0 kcal·mol^(-1)的占94%、小于-7.0 kcal·mol^(-1)的占51%,表明所筛选的潜在活性成分与核心靶点之间具有较好的结合亲和力。结论该研究预测了温性经筋通贴膏治疗类风湿性关节炎的药效物质基础与作用特点,为进一步启发其临床应用及质量控制提供了理论基础。

基于LC-MS/MS测定人体类固醇激素的研究进展

类固醇激素是一类具有环戊烷多氢菲结构的化合物,由细胞色素P450酶催化形成,在调节机体代谢、促进性器官发育等方面起着重要作用。临床上将类固醇激素水平作为肾上腺疾病、精神类疾病等的诊断指标。液相色谱-串联质谱(LC-MS/MS)联用技术因具有高灵敏度、高通量和高专属性的特点,已成为类固醇临床测定的首选方法。本文综述了LC-MS/MS在内源性类固醇激素测定中的应用,特别是在样品前处理、色谱条件和质谱条件优化等方面的研究进展,为临床上类固醇激素的诊断检测提供参考。

瓶内处理技术结合快速LC-MS提高利培酮血药浓度测定效率

目的 评估“瓶内处理”(Bottle-in)技术结合快速LC-MS的方法学特性,并验证其对治疗药物监测技术自动化和标准化的促进作用。方法 选择利培酮及其主要代谢物9-羟利培酮作为研究对象,针对两种血样前处理技术——Bottle-in技术与实验室现行的常规处理(RP)技术,建立并验证相应的LC-MS检测方法。实验设计遵循CLSI EP9-A3指南,对60例服用利培酮的患者血液样本应用两种方法进行利培酮和9-羟利培酮浓度的测定,并记录样本的报告时间。采用Spearman相关性分析、Passing-Bablok回归分析、Bland-Altman一致性检验以及医学决定水平(MDL)预期偏倚分析,对两种方法的检测结果进行相关性和差异性评价。结果 两种前处理技术下的LC-MS方法在测定利培酮和9-羟利培酮血药浓度时,均满足方法学验证的标准。在60例患者的样本中,两组结果均未出现异常值,显示出强烈的相关性(P<0.01)。Passing-Bablok回归模型显示了良好的线性关系。Bland-Altman一致性检验结果表明,两者具有高度一致性。MDL预期偏倚分析进一步证实,两种检测方法的结果未出现显著性偏倚,预期偏倚值(Bc)均在可接受的偏倚限值范围内。Bottle-in技术较RP技术在前处理时间上可节约66.67%,结合快速LC-MS技术对12例患者样本进行检测,全流程检出时间上Bottle-in组较RP组能缩短12.50%的时长。结论 Bottle-in技术凭借其高效的前处理方式,提高了药物监测技术自动化和标准化,可作为替代RP技术的一种有效方法,成为现代临床药学监测中的一项重要进展。

LC-MS/MS法同时测定活血止痛胶囊/片中16种真菌毒素及污染状况分析

目的 建立LC-MS/MS法同时测定活血止痛胶囊/片中黄曲霉毒素B_(1)、B_(2)、G_(1)、G_(2)、M_(1)、M_(2),伏马毒素B_(1)、B_(2)、B_(3),赭曲霉毒素A,玉米赤霉烯酮,脱氧雪腐镰刀菌烯醇,T-2毒素,HT-2毒素,桔青霉毒素,杂色曲霉毒素的含量,并对其污染状况进行分析。方法 以亲水-亲脂HLB固相萃取柱净化作为前处理方式,分析采用Agilent RRHD Eclipse Plus C_(18)色谱柱(2.1 mm×50 mm, 1.8μm);流动相乙腈-水(0.1%甲酸-2 mmol/L甲酸铵),梯度洗脱;体积流量0.3 mL/min;柱温35℃;电喷雾电离源(ESI),正负离子模式,动态多反应离子检测(DMRM)模式。结果 16种真菌毒素在各自范围内线性关系良好(R^(2)>0.999 2),平均加样回收率81.7%~118.0%,RSD 0.9%~13.1%。40批样品中检出黄曲霉毒素B_(1)、G_(1),伏马毒素B_(1)、B_(2),赭曲霉毒素A,杂色曲霉毒素,检出率分别为20%、32.5%、57.5%、25%、42.5%、27.5%,其中黄曲霉毒素B_(1)含量最高,为10.26μg/kg。结论 活血止痛制剂中真菌毒素残留较严重,对人体产生危害的潜在风险较高。

平衡透析结合LC-MS/MS法测定大鼠血浆中游离SN-38浓度及其药代动力学应用

目的 建立大鼠血浆中游离SN-38浓度的LC-MS/MS检测方法。方法 采用平衡透析法模拟SN-38在人体内与血浆蛋白结合的过程,在透析完成后分离出游离SN-38,以[2H5]SN-38为内标,用蛋白沉淀法预处理透析液侧(F侧)样品,取上清液进行LC-MS/MS分析;总SN-38及透析后血浆侧(T侧)SN-38样品的预处理方法与游离SN-38相同;分别考察两种方法的专属性、线性关系、精密度、准确度、提取回收率、基质效应、稳定性。结果F侧SN-38在0.04~80 ng·mL^(-1)内与峰面积线性关系良好(r> 0.99);提取回收率为98.6%~101.6%,基质效应为96.2%~97.2%;日内、日间RSD均<15%,且分别在不同条件下稳定性良好。大鼠血浆样品中的总SN-38在0.5~1000 ng·mL^(-1)内与峰面积线性关系良好(r> 0.99);提取回收率为97.3%~99.5%,基质效应为100.5%~101.2%;日内、日间RSD均<15%,且分别在不同条件下稳定性良好。结论 该方法简单易行、准确、灵敏、专属性好,适用于大鼠血浆中游离SN-38浓度的测定。

基于LC-MS/MS的鹿角方中红景天苷在慢性心力衰竭大鼠心肌组织中的分布

目的分析鹿角方中红景天苷在慢性心力衰竭大鼠心肌组织中的分布。方法45只SPF级雄性Wistar大鼠,6~8周龄,采用简单随机抽样法选取8只作为假手术组,假手术组大鼠只暴露腹主动脉不结扎;其余大鼠行腹主动脉缩窄手术,以血管结扎处明显缩窄示手术成功,术后将存活的32只模型大鼠按体重进行区组随机分组,分为模型组(n=8)、鹿角方低剂量组(1.100 g/kg,n=8)、鹿角方中剂量组(2.200 g/kg,n=8)、鹿角方高剂量组(4.400 g/kg,n=8),药物灌胃干预30周。末次灌胃给药2 h后麻醉大鼠,腹主动脉取血,采集心肌组织,LC-MS/MS法分析不同剂量鹿角方组红景天苷在大鼠左、右心室壁的分布。结果红景天苷在1.195~1195.000 ng/ml范围内线性关系良好(r>0.999),精密度RSD%<15%,准确度为90.817%~106.500%,相对回收率为95.222%~100.814%,基质效应RSD%<15%,样品冰浴放置1 h、前处理后室温放置6 h及自动进样器放置48 h内红景天苷的稳定性良好。红景天苷在右心室壁含量与给药剂量线性拟合值R2为0.983,在中、高剂量鹿角方组中红景天苷在左心室壁的含量分别为右心室壁含量的(47.383±12.156)%、(43.805±9.644)%。结论建立的分析方法具有可行性,红景天苷在慢性心力衰竭大鼠左、右心室分布存在差异。

LC-MS/MS法测定大鼠血浆中S,S,S-三丁基三硫代磷酸酯质量浓度及其毒物动力学研究

目的 建立LC-MS/MS法测定大鼠血浆中S,S,S-三丁基三硫代磷酸酯的质量浓度,并用于大鼠体内的毒物动力学研究。方法 采用沉淀蛋白法进行血浆样品前处理,以丙酸倍氯米松为内标。色谱柱为Agilent Zorbax SB C_(18)(50 mm×2.1 mm, 3.5μm)柱,流动相为水(含体积分数0.1%甲酸)-乙腈/甲醇(体积比1∶1),梯度洗脱,流速为0.8 mL·min^(-1)。质谱检测采用ESI源,正离子化方式,多反应监测模式(MRM)进行扫描检测。结果 血浆中S,S,S-三丁基三硫代磷酸酯线性范围为2~800μg·L^(-1),线性良好(r≥0.99),批内、批间RSD均在±15%内,准确度在85%~115%内。高、中、低质量浓度总体提取回收率为89.0%,变异系数为1.1%。结论 本方法适用于大鼠血浆中S,S,S-三丁基三硫代磷酸酯质量浓度的准确测定和动力学研究。

LC-MS在手性农药对映体分析中的应用

目前使用的农药中,手性农药占40%。手性农药具有一个或多个手性中心,同时也具有多对对映异构体,它们在生物活性、生态毒性和环境行为等方面表现出对映选择性差异。利用液相色谱–质谱联用技术(LC-MS)可以分析出如活性高、毒性低的优势对映异构体,推动农药单体的生产和推广,对食品和环境安全具有重要意义。本文综述了LC-MS在手性农药杀菌剂、杀虫剂和除草剂对应异构体分析中的应用,旨在为农药单体使用提供依据。

LC-MS/MS法测定鲤鱼中苦参碱和氧化苦参碱

建立基于前处理技术结合液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)对鲤鱼基质中苦参碱和氧化苦参碱残留量测定的分析方法.样品采用乙腈均质提取的萃取方式,用硫酸钠作为除水剂,样品经过C18色谱柱分离,以水-乙腈为流动相,基质匹配标准曲线外标法定量.苦参碱和氧化苦参碱在质量浓度范围1—50 ng·mL^(−1)内,具有良好的线性关系,相关系数R^(2)均大于0.99.苦参碱方法检出限为0.21 ng·mL^(−1),定量限为0.69 ng·mL^(−1);氧化苦参碱方法检出限为0.17 ng·mL^(−1),定量限为0.52 ng·mL^(−1).添加浓度水平1.0、2.0、5.0 ng·mL^(−1),平均回收率为72.5%—108.7%,相对标准偏差(relative standard deviation,RSD,n=6)为4.2%—8.2%.苦参碱和氧化苦参碱的基质效应均表现为抑制.该方法前处理方法简单,灵敏度高,稳定性好,适合鲤鱼基质苦参碱和氧化苦参碱残留量的测定,同时为后续同类样品检测提供参考,也为今后相关标准制定提供数据积累.

缬沙坦类药物中相关杂质的LC-MS/MS测定

采用L C-M S/M S方法建立了缬沙坦类药物中相关杂质的测定,使用Discovery^(®)HS F5,(5μm particle size,L×I.D.15 cm×4.6 mm)色谱柱,流动相A为0.1%甲酸水溶液;流动相B为0.1%甲酸甲醇溶液,梯度洗脱,流速为0.40 mL/min,离子化模式为:ESI+,多反应监测模式(MRM)进行定性分析;基质外标法进行定量分析,得到缬沙坦类药物中相关杂质的检出限为10.0μg/kg;定量限为20.0μg/kg,在线性浓度范围为10~100μg/L之间有良好的线性关系相关系数均大于0.999,加标回收率为72.3%~86.9%,相对标准偏差(RSD)为4.7%~8.9%。本方法对于缬沙坦类药物中有关物质的检测分析结果准确率高,可靠性强,适合检测缬沙坦类药物中有关物质的残留量。

Verification and Validation of High-Resolution Inviscid and Viscous Conical Nozzle Flows

Capturing elaborated flow structures and phenomena is required for well-solved numerical flows.The finite difference methods allow simple discretization of mesh and model equations.However,they need simpler meshes,e.g.,rectangular.The inverse Lax-Wendroff(ILW)procedure can handle complex geometries for rectangular meshes.High-resolution and high-order methods can capture elaborated flow structures and phenomena.They also have strong mathematical and physical backgrounds,such as positivity-preserving,jump conditions,and wave propagation concepts.We perceive an effort toward direct numerical simulation,for instance,regarding weighted essentially non-oscillatory(WENO)schemes.Thus,we propose to solve a challenging engineering application without turbulence models.We aim to verify and validate recent high-resolution and high-order methods.To check the solver accuracy,we solved vortex and Couette flows.Then,we solved inviscid and viscous nozzle flows for a conical profile.We employed the finite difference method,positivity-preserving Lax-Friedrichs splitting,high-resolution viscous terms discretization,fifth-order multi-resolution WENO,ILW,and third-order strong stability preserving Runge-Kutta.We showed the solver is high-order and captured elaborated flow structures and phenomena.One can see oblique shocks in both nozzle flows.In the viscous flow,we also captured a free-shock separation,recirculation,entrainment region,Mach disk,and the diamond-shaped pattern of nozzle flows.

基于LC-MS/MS技术的水蛭配方颗粒中7种碱基和核苷成分分析方法的建立

本文建立了一种使用岛津超高效液相色谱仪Nexera X2和三重四极杆质谱仪LCMS-8050联用测定水蛭配方颗粒中7种碱基和核苷成分的分析方法.水蛭配方颗粒以10%甲醇50℃超声提取30 min,MRM正负模式同时检测.以Discovery■HS F5-3色谱柱进行分离,流动相为0.15%甲酸水溶液和甲醇,10 min内完成梯度洗脱.本方法采用外标法定量,7种化合物在相应的浓度范围内线性关系良好,判定系数(R^(2))均大于0.996,定量限在0.42—3.94μg·g^(-1)之间. 10 ng·mL^(-1)的混合标准品溶液连续进样6次,待测化合物峰面积RSD均小于6%,精密度良好.平行6份加标回收试验,7种化合物平均回收率在87.09%—105.81%之间,RSD%在1.35%—4.70%之间.残留实验结果为阴性.该方法准确可靠,可为水蛭配方颗粒的质量控制提供参考依据.

Push forward LC-MS-based therapeutic drug monitoring and pharmacometabolomics for anti-tuberculosis precision dosing and comprehensive clinical management

The spread of tuberculosis(TB),especially multidrug-resistant TB and extensively drug-resistant TB,has strongly motivated the research and development of new anti-TB drugs.New strategies to facilitate drug combinations,including pharmacokinetics-guided dose optimization and toxicology studies of first-and second-line anti-TB drugs have also been introduced and recommended.Liquid chromatography-mass spectrometry(LC-MS)has arguably become the gold standard in the analysis of both endo-and exo-genous compounds.This technique has been applied successfully not only for therapeutic drug monitoring(TDM)but also for pharmacometabolomics analysis.TDM improves the effectiveness of treatment,reduces adverse drug reactions,and the likelihood of drug resistance development in TB patients by determining dosage regimens that produce concentrations within the therapeutic target window.Based on TDM,the dose would be optimized individually to achieve favorable outcomes.Pharmacometabolomics is essential in generating and validating hypotheses regarding the metabolism of anti-TB drugs,aiding in the discovery of potential biomarkers for TB diagnostics,treatment monitoring,and outcome evaluation.This article highlighted the current progresses in TDM of anti-TB drugs based on LC-MS bioassay in the last two decades.Besides,we discussed the advantages and disadvantages of this technique in practical use.The pressing need for non-invasive sampling approaches and stability studies of anti-TB drugs was highlighted.Lastly,we provided perspectives on the prospects of combining LC-MS-based TDM and pharmacometabolomics with other advanced strategies(pharmacometrics,drug and vaccine developments,machine learning/artificial intelligence,among others)to encapsulate in an all-inclusive approach to improve treatment outcomes of TB patients.

HPLC-DAD法结合LC-MS/MS法检测艾绒和艾条中非法添加的色素

目的通过HPLC-DAD法结合LC-MS/MS法检测艾绒和艾条中非法添加的金胺O和酸性黄36。方法HPLC-DAD分析采用WelchMaterialsEclipseXB-C_(18)色谱柱(4.6mm×250mm,5μm);流动相乙腈-0.01mol/L乙酸铵(含0.1%甲酸)(35∶65);体积流量1.0mL/min;柱温35℃;检测波长425nm;采用LC-MS/MS法对所检出的阳性样品进行验证。结果金胺O和酸性黄36在各自范围内线性关系良好(r>0.9995),平均加样回收率分别为94.8%、96.2%,RSD分别为1.1%、0.26%。67批样品中有7批存在非法染色嫌疑,阳性检出率为10.4%。结论该方法准确灵敏,可用于艾绒和艾条中非法添加色素的检测,并为相关国家标准的提高提供参考。

Accurate Source-Receiver Positioning Method for a High-Resolution Deep-Towed Multichannel Seismic Exploration System

The near-seabed multichannel seismic exploration systems have yielded remarkable successes in marine geological disaster assessment,marine gas hydrate investigation,and deep-sea mineral exploration owing to their high vertical and horizontal resolution.However,the quality of deep-towed seismic imaging hinges on accurate source-receiver positioning information.In light of existing technical problems,we propose a novel array geometry inversion method tailored for high-resolution deep-towed multichannel seismic exploration systems.This method is independent of the attitude and depth sensors along a deep-towed seismic streamer,accounting for variations in seawater velocity and seabed slope angle.Our approach decomposes the towed line array into multiline segments and characterizes its geometric shape using the line segment distance and pitch angle.Introducing optimization parameters for seawater velocity and seabed slope angle,we establish an objective function based on the model,yielding results that align with objective reality.Employing the particle swarm optimization algorithm enables synchronous acquisition of optimized inversion results for array geometry and seawater velocity.Experimental validation using theoretical models and practical data verifies that our approach effectively enhances source and receiver positioning inversion accuracy.The algorithm exhibits robust stability and reliability,addressing uncertainties in seismic traveltime picking and complex seabed topography conditions.

基于HPLC与LC-MS/MS分析食品组合物桑瓜饮的化学成分

解析具有调节血糖功能的食品组合物桑瓜饮(Sang-Gua-Yin,SGY)的成分。使用高效液相色谱(High Performance Liquid Chromatography,HPLC)归属桑叶总生物碱组分、苦瓜总皂苷组分、葛根总黄酮组分的色谱峰,高效液相色谱-蒸发光散射器(High Performance Liquid Chromatography-Evaporative light Scattering Detector,HPLC-ELSD)与液相色谱-串联质谱法(Liquid Chromatography-Tandem Mass Spectrometry,LC-MS/MS)分析组合物桑瓜饮中的化学成分。对食品组合物桑瓜饮的色谱峰进行归属,标定了11个色谱峰,其中7种成分属于葛根总黄酮,3种成分属于苦瓜总皂苷,1种成分属于桑叶总生物碱;对16个化学成分进行了鉴定,分别为1-DNJ、苦瓜苷A、苦瓜苷K、葛根素、6′′-O-acetyldaidzin、pueroside D、染料木苷、大豆苷、大豆苷元、3′-羟基葛根素、3′-甲氧基葛根素、3′-氢化葛根素木糖苷、葛根素-7-木糖苷、葛根素-6′′-O-木糖苷、puerarin-7-O-glucoside、葛根素-4′-O-β-D-葡萄糖苷。该研究提示食品组合物桑瓜饮成分选择1-DNJ、苦瓜苷A与葛根素作为评价指标,为食品组合物桑瓜饮的后续开发利用提供科学依据。

Investigating the relationship between intracranial atherosclerotic plaque remodelling and diabetes using high-resolution vessel wall imaging

BACKGROUND Intracranial atherosclerosis,a leading cause of stroke,involves arterial plaque formation.This study explores the link between plaque remodelling patterns and diabetes using high-resolution vessel wall imaging(HR-VWI).AIM To investigate the factors of intracranial atherosclerotic remodelling patterns and the relationship between intracranial atherosclerotic remodelling and diabetes mellitus using HR-VWI.METHODS Ninety-four patients diagnosed with middle cerebral artery or basilar artery INTRODUCTION Intracranial atherosclerotic disease is one of the main causes of ischaemic stroke in the world,accounting for approx-imately 10%of transient ischaemic attacks and 30%-50%of ischaemic strokes[1].It is the most common factor among Asian people[2].The adaptive changes in the structure and function of blood vessels that can adapt to changes in the internal and external environment are called vascular remodelling,which is a common and important pathological mechanism in atherosclerotic diseases,and the remodelling mode of atherosclerotic plaques is closely related to the occurrence of stroke.Positive remodelling(PR)is an outwards compensatory remodelling where the arterial wall grows outwards in an attempt to maintain a constant lumen diameter.For a long time,it was believed that the degree of stenosis can accurately reflect the risk of ischaemic stroke[3-5].Previous studies have revealed that lesions without significant luminal stenosis can also lead to acute events[6,7],as summarized in a recent meta-analysis study in which approximately 50%of acute/subacute ischaemic events were due to this type of lesion[6].Research[8,9]has pointed out that the PR of plaques is more dangerous and more likely to cause acute ischaemic stroke.Previous studies[10-13]have found that there are specific vascular remodelling phenomena in the coronary and carotid arteries of diabetic patients.However,due to the deep location and small lumen of intracranial arteries and limitations of imaging techniques,the relationship between intracranial arterial remodelling and diabetes is still unclear.In recent years,with the development of magnetic resonance technology and the emergence of high-resolution(HR)vascular wall imaging,a clear and multidimensional display of the intracranial vascular wall has been achieved.Therefore,in this study,HR wall imaging(HR-VWI)was used to display the remodelling characteristics of bilateral middle cerebral arteries and basilar arteries and to explore the factors of intracranial vascular remodelling and its relationship with diabetes.

In vivo pilot study into superficial microcirculatory characteristics of colorectal adenomas using novel high-resolution magnifying endoscopy with blue laser imaging

BACKGROUND No studies have yet been conducted on changes in microcirculatory hemody-namics of colorectal adenomas in vivo under endoscopy.The microcirculation of the colorectal adenoma could be observed in vivo by a novel high-resolution magnification endoscopy with blue laser imaging(BLI),thus providing a new insight into the microcirculation of early colon tumors.AIM To observe the superficial microcirculation of colorectal adenomas using the novel magnifying colonoscope with BLI and quantitatively analyzed the changes in hemodynamic parameters.METHODS From October 2019 to January 2020,11 patients were screened for colon adenomas with the novel high-resolution magnification endoscope with BLI.Video images were recorded and processed with Adobe Premiere,Adobe Photoshop and Image-pro Plus software.Four microcirculation parameters:Microcirculation vessel density(MVD),mean vessel width(MVW)with width standard deviation(WSD),and blood flow velocity(BFV),were calculated for adenomas and the surrounding normal mucosa.RESULTS A total of 16 adenomas were identified.Compared with the normal surrounding mucosa,the superficial vessel density in the adenomas was decreased(MVD:0.95±0.18 vs 1.17±0.28μm/μm2,P<0.05).MVW(5.11±1.19 vs 4.16±0.76μm,P<0.05)and WSD(11.94±3.44 vs 9.04±3.74,P<0.05)were both increased.BFV slowed in the adenomas(709.74±213.28 vs 1256.51±383.31μm/s,P<0.05).CONCLUSION The novel high-resolution magnification endoscope with BLI can be used for in vivo study of adenoma superficial microcirculation.Superficial vessel density was decreased,more irregular,with slower blood flow.

LC-MS/MS法测定桃红四物汤中芍药苷的含量

目的建立LC-MS/MS测定桃红四物汤中芍药苷含量的方法。方法色谱分离采用Agilent Eclipse Plus C_(18)(2.1 mm×50 mm,5μm)色谱柱,流动相为甲醇和水(含0.1%甲酸),梯度洗脱。质谱采集选用ESI负离子及多反应监测模式。结果芍药苷在0.1~50μg/ml范围内线性关系良好,专属性、回收率、精密度、均一性均符合要求。结论本法专属性强、灵敏度高、分析时间短,可作为桃红四物汤中芍药苷的含量测定。