目的 采用超高效液相色谱串联四级杆飞行时间质谱联用技术对益气健脾颗粒中化学成分进行初步鉴定和归属分类.方法 采用YMC-Pack ODS-A色谱柱(250 mm×4.6 mm,5 μm),以0.2％甲酸水-甲醇为流动相体系,梯度洗脱,进样量8μL,体积流量1.0 mL/min,在正、负离子模式下对色谱流出物进行质谱检测.结果 通过与对照品比对、自建数据库匹配,结合文献报道,从益气健脾颗粒中鉴定出130个化学成分,包括54个黄酮类、22个萜类、20个含氮化合物、14个香豆素类、12个有机酸类,还有8个醇苷类、鞘脂类等其他成分.结论 建立的定性分析方法能系统、快速地对益气健脾颗粒中的成分进行识别,为益气健脾颗粒的质量控制和研究药效物质基础提供重要依据.

目的:研究青礞石对戊四氮(PTZ)点燃癫痫大鼠脑组织、血浆中金属元素的影响,探讨青礞石可能的效应物质基础.方法:采用PTZ点燃法建立癫痫大鼠模型,运用电感耦合等离子体质谱法(ICP-MS)和电感耦合等离子体发射光谱法(ICP-OES)测定空白组、模型组、卡马西平组(0.1g·kg-1)和青礞石组(2 g·kg-1)大鼠脑组织、血浆中的金属元素含量,实验数据用SPSS 18.0软件进行统计学分析.结果:与空白组比较,模型组大鼠脑组织中Sr,Sb,Ba含量明显上升(P＜0.05,P＜0.01);Zn,Fe,Cu,K,Li,Co,Sn,Pb含量明显下降(P＜0.05,P＜0.01).与模型组比较,青礞石组大鼠脑组织中Zn,Fe,K,Li,Co,As,Pb含量明显上升(P＜0.05,P＜0.01);Sr,Sb含量显著下降(P＜0.01).说明青礞石对大鼠脑组织中金属元素含量向正常水平的调节具有积极作用,干预效果明确,且总体效果优于卡马西平组.与空白组比较,模型组大鼠血浆中K,Sr,Cd含量明显上升(P＜0.05);Li,Al,Ti,Cr含量明显下降(P＜0.05).与模型组比较,青礞石组大鼠血浆中Ca,K,Li,Al,V含量明显上升(P＜0.05,P＜0.01);Fe,Ti,Sr,Cd含量明显下降(P＜0.05,P＜0.01).各组间金属元素相关性分析显示,大鼠脑组织中有17对元素存在显著正相关性,2对元素存在显著负相关性,大鼠血浆组织中有8对元素存在显著正相关性,6对元素存在显著负相关性.结论:以Zn,Fe,K,Li,Co,As,Pb,Sr,Sb,Ca,Al,V,Ti,Cd为代表的金属元素群可能是青礞石干预PTZ点燃癫痫模型大鼠的效应物质基础,作用机制可能与这些金属元素群干预影响神经递质的释放及神经元的电平衡、调节离子(Na+,K+,Ca2+等)通道失常诱发的异常同步放电及干预癫痫相关代谢通路等有关,使兴奋与抑制活动相互牵制,最终达到神经元、细胞电平衡等趋于正常生理状态.青礞石组的干预作用总体优于卡马西平组.

随着我国经济的发展,高校分析测试中心不断壮大.分析测试中心是高校建设的重要部分,要为学校教学科研,培养高素质创新型人才提供支持,应实现大型分析测试仪器设备资源共享.要使高校分析测试中心走上可持续发展道路,使其适应科技发展形势,充分发挥高校分析测试中心教学等多种功能.本文对高校分析测试中心服务于高校教育科研的作用进行分析,阐述高校分析测试中心建设中的问题,从建立测试基金、开放仪器使用等方面提出建议.

目的:通过青礞石干预戊四氮(PTZ)点燃癫痫大鼠的脑组织代谢组学研究,探讨青礞石治疗癫痫可能的作用机制.方法:运用PTZ点燃法建立大鼠癫痫动物模型,实验分为空白组、模型组、卡马西平组、青礞石组.通过超高效液相色谱-四极杆飞行时间质谱法(UPLC/Q-TOF-MS)技术检测脑组织样品,利用偏最小二乘法-判别分析(PLS-DA)和SPSS 18.0软件等方式对实验结果进行统计分析.结果:建立了大鼠脑组织代谢指纹图谱、代谢轮廓图,显示各组代谢轮廓发生了明显的变化,各组间均能很好地分开,并且青礞石组较卡马西平组有更靠近空白组的趋势.筛选出了7个差异代谢物,包括磷脂酰丝氨酸(PS)(18∶0/18∶0),L-谷氨酸,二十二碳六烯酰基乙醇酰胺,花生四烯酸,葡糖鞘氨醇,胆甾烷-3,7,12,24,25-五醇,溶血磷脂酰胆碱(LysoPC)(P-18∶0).除二十二碳六烯酰基乙醇酰胺和LysoPC(P-18∶0)外,青礞石对其他5个差异代谢物均有显著性干预调节作用.影响PTZ点燃大鼠发生代谢紊乱的可能代谢通路有12条,较为重要的代谢通路有3条,即D-谷氨酰胺和D-谷氨酸代谢,丙氨酸、天冬氨酸和谷氨酸代谢以及花生四烯酸代谢,其中又以D-谷氨酰胺和D-谷氨酸代谢最为重要.结论:从脑组织代谢组学分析来看,青礞石对PTZ癫痫大鼠具有明确的干预作用,这可能与其干预以上差异代谢物含量及相关代谢通路有关,可减少兴奋性神经递质对脑组织神经元的毒性作用以及抑制脑组织炎症的发展以维持脑细胞的生物学功能而减缓癫痫发生.

目的 比较不同饮片中的焦香味醛类物质含量变化,寻求薏苡仁饮片炮制的过程监控指标.方法 对薏苡仁的生品饮片、清炒饮片、麸炒饮片和从外表面刮下来的表层焦黄物质进行GC-MS测定,GC-MS色谱条件:色谱柱为HP-5(MS)毛细管柱,柱温为50℃升至230℃(4℃/min);进样口温度240℃,载气用高纯He气,顶空进样时间1次1 min,色谱柱分流比25:1.结果 麸炒薏苡仁饮片中3-甲基和2-甲基丁醛的含量明显高于生品饮片和清炒饮片,约为生品饮片的2倍,而清炒品含量几乎不变.结论 此方法简便易行,麸炒产生的焦香味醛类物质可以作为麸炒炮制的过程监控指标.

OBJECTIVE To identify the main chemical components in herbal pair:Astragali Radix and Salviae Miltior-rhizae by UFLC-Q-TOF/MS.METHODS Thermo BDS C1 8(3 μm,1 50 mm×2.1 mm) column was employed for the separa-tion with acetonetrile-water(0.1% formic acid)as mobile phase using a gradient elution program.The flow rate was set as 0. 3 mL/min,the temperature of column was 40 ℃ with injection volume of 5 μL.Electrospray ionization(ESI)-Q-TOF/MS in negative ion mode was performed to obtain the MS spectra with full mass scan m/z ranged from 100 to 1 500.Chemicals were identified based on the retention time,high-resolution mass information,MS/MS fragmentation behaviors and standards.RE-SULTS 28 components were identified or tentatively characterized in herbal pair:Astragali Radix and Salviae Miltiorrhizae, including 1 5 components in Salviae Miltiorrhizae ,1 1 compounds in Astragali Radix ,and 2 unknown compounds.And these chemicals could be classified as triterpenes,organic acids,flavonoids and quinines.CONCLUSION This method can rapidly and accurately identify the main compounds in herbal pair:Astragali Radix and Salviae Miltiorrhizae ,which can help us for the quality control and further phytochemical studies of Astragali Radix and Salviae Miltiorrhizae .in traditional Chinese medicine.

目的 建立UPLC法分析藤黄Garcinia hanburyiHook.f.及其炮制品(高压制、豆腐制、清水制)中藤黄烯酸、表藤黄烯酸、藤黄酸、新藤黄酸含有量的变化.方法 该植物乙腈提取液的分析采用UPLC HSS T3色谱柱(100 mm×2.1mm,1.8μm);流动相乙腈-0.1％甲酸(80∶20);体积流量0.3 mL/min;检测波长360 nm.结果 4种成分在各自范围内均呈良好的线性关系(r ＞0.999 3),平均加样回收率100.9％～103.0％(RSD＜ 3.0％).炮制后,藤黄酸和新藤黄酸的含有量均有所下降,分别在清水、豆腐制品中最低.同时,新生成了藤黄烯酸和表藤黄烯酸,两者含有量在清水制品中最高,高压制品中最低.结论 清水制法有利于藤黄烯酸和表藤黄烯酸的生成.

ABSTRACT:OBJECTIVE To study the excretion of Liguzinediol and its metabolites in rats by UPLC-PDA method.METH-ODS Six SD rats were administered intravenously at a dose of 10 mg∕kg.Its urine,bile and feces were collected according to certain time points.The samples were treated by methanol and the supernatant was dried by N2 ,then dissolved by mobile phase.Liguzinediol and its metabolites in urine,bile and feces were determinated by UPLC-PDA.Conversion factor was con-firmed through the determination of UV absorption coefficient and molecular weight of prototype drug together with its metab-olites.Then the cumulative excretion of Liguzinediol in rats(Dose%)was calculated.RESULTS There were slight differences in the excretion process between female and male rats.The Dose% of Liguzinediol and its main metabolites in female rats u-rine,bile and feces respectively were 47.94%,1 6.67% and 0.648%,and the total Dose% was 65.26%.The Dose% of Ligu-zinediol and its main metabolites in male rats urine,bile and feces respectively were 35.00%,20.37% and 1.1 56%,and the total Dose% was 56.53%.CONCLUSION The UPLC-PDA method with the addition of conversion factor can be used to ex-plore the material balance of Liguzinediol in rats,and provide experimental evidence for clinical research.

目的:建立液质联用技术同时测定不同产地淡豆豉中38种核苷和氨基酸类含量的方法.方法:采用超快速液相色谱和三重四极杆.线性离子阱串联质谱以及亲水色谱柱(2.1 mm×100 mm,3.5 μm),流动相0.2％甲酸水-0.2％甲酸乙腈梯度洗脱,流速0.6 mL· ain-,采用电喷雾正离子化及多反应监测模式(MRM),对安徽、江苏、河南3个产区不同采收期共8个批次淡豆豉中的22种氨基酸类和16种核苷类成分进行含量测定;并对结果进行PCA-DA聚类分析及t检验.结果:所建方法使淡豆豉中22种氨基酸类和16种核苷类成分得到较好分离,浓度与峰面积呈良好的线性关系,加样回收率在93.74％～104.32％,RSD在0.6％ ～3.5％;8个批次样品基本可以测得22种氨基酸类和16种核苷类成分,各批次间核苷与氨基酸的含量都有明显差异,总氨基酸质量分数在7.241～34.21 mg·g-1,总核苷质量分数在14.21 ～82.53 mg·g-1;不同产地样品的氨基酸含量高低排序为安徽产＞江苏产＞河南产,不同产地样品的核苷含量高低排序为江苏产与安徽产＞河南产,同-产地贮存时间短的样品总氨基酸和总核苷含量也高于贮存时间长的.结论:该方法适用于38种核苷和氨基酸类成分含量的同时测定,比较了不同产地淡豆豉的差异性,在一定程度上反应了不同产区间淡豆豉的质量优劣,为后续药效活性研究提供参考.

Objective To establish and identify the HPLC-PDA fingerprint of Atractylodis Macrocephalae Rhizoma (AMR) and provide a reference for the comprehensive control of the quality of AMR.Methods AMR was extracted with 70％ methanol by sonicating for 60 min.The analysis of AMR extract was performed on Inertsil~ ODS-SP column (150 mm × 4.6 mm,5 μm),column temperature was maintained at 40 ℃,flow rate was 1.0 mL/min,and detector was Waters 2998 UV detector with detection wavelength 235 nm.Mobile phase was acetonitrile (B)-water (A) with the elution gradient 0-10 min,30％-45％ B,10-25 min,45％ B,25-50 min,45％-70％ B,50-55 min,70％ B,55-62 min,70％-30％ B,62-75 min,30％ B.Time-of-flight mass spectrometer (TOF/MS) and electro-spray ion (ESI) source were used for the qualitative analysis in a positive ion mode,and mass scan range was m/z 50-1 500.Results Comparing and fitting the peaks of AMR from different habitats (Zhejiang,Anhui,and Hunan Provinces),the HPLC-PDA fingerprint was set up with six common peaks,and they were identified by UFLC-Q-TOF/MS as 5-(hydroxymethyl)-2-furaldehyde,atractylenolide Ⅲ,atractylenolide Ⅰ,atractylenolide Ⅱ,atractylenolide Ⅵ,and biatractylenolide.System suitability,extraction,and chromatographic conditions of AMR were optimized.RSD of accuracy,stability and repeatability was all less than 2％.Measuring ten batches and fitting fingerprint similarity,the values were all greater than 0.95.Conclusion The HPLC fingerprint can be used as standard uniformity and stability of quality control methods for AMR slice.

目的 比较研究不同种属间liguzinediol的体外代谢产物.方法 建立liguzinediol及其体外代谢产物的LC-MS/MS检测方法,采用肝微粒体温孵法研究liguzinediol在大鼠、犬、猴、人等多种属肝微粒体中的代谢产物.结果 liguzinediol在肝脏可发生Ⅰ相和Ⅱ相代谢,并且在大鼠、犬、猴、人肝微粒体温孵体系中均孵育有氧化产物和葡萄糖醛酸结合产物.结论 liguzinediol在大鼠、犬和猴等动物的肝微粒体中的Ⅰ相和Ⅱ相代谢产物与人肝微粒体基本一致,该研究结果可为liguzinediol临床前安全性评价的实验动物选择提供依据.

目的:利用超快速液相-四级杆-飞行时间串联质谱（UFLC/Q-TOF-MS）结合主成分分析法考察人参-黄连共煎前后人参皂苷类成分的变化。方法:采用UPLC T3 C18色谱柱（2.1 mm×100 mm,1.8μm）,流动相0.3%甲酸-0.3%甲酸乙腈梯度洗脱,负离子模式下采集质谱数据,应用Markview1.2.1等软件进行主成分分析（PCA）,以黄连水煎液为空白,比较人参水煎液与人参-黄连共煎中人参皂苷类成分的变化。结果:3种溶液中发现10个差异性人参皂苷类化合物,其中齐墩果酸和2个未知化合物含量显著上升,20-葡萄糖Rf和人参皂苷Rf,Ra3,Rb1,Ra2,Rb3,Rs2含量显著下降。结论:负离子模式下方法能很好区分共煎前后人参皂苷类成分的变化,提示人参皂苷类成分水解生成的齐墩果酸型苷元可能是人参与黄连共煎后的物质基础。

目的 建立荨麻中3,4-二香草基四氢呋喃的含量测定的方法.方法 采用Kromasil C18色谱柱(4.6mm×150 mm,5 μm),柱温为40℃;以甲醇-水(0.05％三氟乙酸)(55∶45)为流动相,流速为1.0mL·min-1;检测波长为230 nm.结果 在选定的色谱条件下,3,4-二香草基四氢呋喃在10.0～50.0μg·mL-1,浓度与峰面积线性关系良好(r=0.9999),低、中、高浓度平均回收率在96.5％～100.8％,RSD均＜2.5％.结论 本方法操作简便,结果可靠,重现性好,适用于荨麻中3,4-二香草基四氢呋喃的含量测定,可用于荨麻的质量控制.

以南京中医药大学药学院分析测试中心服务于实验教学为例，对测试中心服务于实验教学过程中面向群体、开放形式、服务理念的必要性和改革方式两方面进行分析与讨论，指出分析测试中心作为高校重要组成部分，必须充分认识到实验教学的重要性，并对其进行科学的管理，充分发挥实验教学在人才培养和教育过程中的功能和作用，真正做到更好地为教学工作服务，培养出合格人才。

liguzinediol是一种毒性较小[1],具有心脏安全性,可用于治疗急性心衰的化合物.它通过影响肌浆网钙释放,增加大鼠在体和离体的心脏收缩力[2-3],对正常大鼠及其离体心脏起到较好的正性肌力作用[4-5].前期对liguzinediol在大鼠体内的药代动力学、♀♂差异及药物代谢进行了研究报道[6-8].根据一类新药研制的要求,比格犬体内的药代动力学研究对指导临床具有更为重要的意义[9-10],本文首次研究了比格犬静注liguzinediol后的血浆药代动力学,为liguzinediol的进一步开发和临床研究提供了必要的实验依据.

目的 探讨一种快速同时测定抗601合剂中黄芩苷及绿原酸含量的方法.方法 采用超高效液相色谱(UPLC)法,色谱柱为Waters ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8 μm),流动相为甲醇-0.3％甲酸水溶液(梯度洗脱),流速0.3 mL/min,检测波长:280 nm.结果 黄芩苷在28.8～288μg/mL范围内呈良好的线性关系(r=0.999 9),绿原酸在6.6～66 μg/mL范围内呈良好的线性关系(r=0.999 9).平均加样回收率分别为98.71％(n=6)、98.27％(n=6),RSD分别为0.66％和0.95％.结论 所用方法快速、简便、准确,可为抗601合剂的质量控制提供依据.

AIM To use an ultra-flow liquid chromatography couple with quadrupole-time-of-flight mass-spectrometry( UFLC / Q-TOF-MS)-based chemical analysis to evaluate the chemical constituents of Atractylodes chinensis( DC.) Koidz. fried with wheat bran. METHOD The chromatographic separation was performed on an ACQUITY UPLC T3 C18column with water-acetonitrile as mobile phase in a gradient elution mode. The mass spectrometer equipped with electrospray ionization source was used as detector under the positive ion mode. The difference of Atractylodes chinensis( DC.) Koidz,processing with and without bran-frying as compared with bran as( blank) and were classfied by principal component analysis( PCA) with Markerview software. RESULTS Under the condition of positive ion mode,PCA method could distinguish the bran intervention. After being processed with bran-frying,the contents of atractyloside A,atractylenolide Ⅰ,atractylenolide Ⅱ,and an unknown compound increased,while the contents of α-gurcumene,hinesol,atractylenolide Ⅲ,and atractylodin decreased. CONCLUSIONS Bran-frying makes the dehydration and dehydrogenation of atractylenolide Ⅲ and increase the conversion of actracty lenolide I and II related to the fortification of the spleen.

Objective: To establish a simple and sensitive LC-MS/MS method for determining liguzinediol and study the pharmacokinetics of liguzinediol in male and female rats,respectively.Methods: Measurement of liguzinediol was performed by positive ion electrospray ionization in multiple reaction monitoring mode,and monitoring the transitions m/z 169.2→122.2 for liguzinediol and m/z 195.2→110.2 for caffeine,respectively.Separation of liguzinediol and caffeine in plasma sample was carried out on Shim-pack XR-ODS column(50 mm×2.0 mm,2.2 μm) eluting with a gradient mobile phase system at a flow rate of 0.4 mL·min-1.The sample injection volume was 2 μL and the column temperature was maintained at 40 ℃.Seventy-two Sprague-Dawley rats were divided into 6 male groups and 6 female groups.Three male groups and three female groups were administrated with an oral dose of 5,10 and 20 mg·kg-1,respectively.Another three male groups and three female groups were administrated with an intravenous dose of 5,10 and 20 mg·kg-1,respectively.The pharmacokinetic parameters were calculated by DAS 2.1 software.Results: Good linearity was obtained over the range of 10~20 000 ng·mL-1,and the correlation coefficient was better(r=0.999 6).They met the requirements of the analysis of biological samples with RSD of the intra-and inter-day precisions(15%).Disparity was found between male and female rats in the pharmacokinetic parameters.Conclusion: The developed method is successfully applied to the pharmacokinetic study in rats.