基于~1H NMR技术的奶牛Ⅰ型和Ⅱ型酮病血浆代谢谱分析

【目的】运用代谢组学中1H NMR技术方法筛选出Ⅰ型酮病、Ⅱ型酮病与健康对照组之间血浆差异性代谢物。【方法】选取产后7—28 d,平均胎次为2—3胎的实验奶牛50头。根据血糖(Glc)、β-羟丁酸(BHBA)和游离脂肪酸(NEFA)的含量与临床发病特点分为Ⅰ型酮病、Ⅱ型酮病与健康对照组,其中Ⅰ型酮病20头,Ⅱ型酮病为20头,健康对照组为10头。当患病牛血中BHBA>1.20 mmol?L-1,Glc<2.50 mmol?L-1,NEFA>0.50 mmol·L-1时,被认为患I型酮病;当患病牛血浆中BHBA>1.20 mmol?L-1,Glc>2.80 mmol?L-1,NEFA>0.50 mmol?L-1时,被认为患II型酮病;当奶牛血中BHBA<1.00 mmol?L-1,Glc>3.75 mmol?L-1,NEFA<0.40 mmol?L-1时,被认为健康对照组。运用代谢组学中1H NMR技术对实验奶牛的血浆代谢物分析,获得相应的代谢图谱,并结合多元统计分析中的主成分分析(PCA)、正交偏最小二乘判别分析(OPLS-DA)的模式判别,从而寻找潜在的生物标记物。【结果】通过1H NMR分析,Ⅰ型酮病、Ⅱ型酮病与健康对照的代谢图谱差异明显,3组代谢产物各自聚集,分散区域显著。Ⅱ型酮病与健康对照比较,获得7种血浆差异代谢物,主要为丙氨酸、赖氨酸、β-羟丁酸、丙酮、乳酸等,其中血浆中β-羟丁酸、丙酮、乳酸浓度升高;丙氨酸、赖氨酸、酪氨酸、肌酸浓度呈现下降。Ⅰ型酮病与健康对照组比较,获得19种血浆差异代谢物,主要为酪氨酸、苯丙氨酸、肌酸、β-羟丁酸、丙酮等,其中β-羟丁酸、丙酮浓度升高;酪氨酸、苯丙氨酸、赖氨酸、组氨酸、丙氨酸、肌酸、肌醇、β-葡萄糖、谷氨酰胺、谷氨酸、柠檬酸、α-葡萄糖、甲酸、甘氨酸、O-乙酰葡萄糖胺、磷酸胆碱浓度呈现下降。Ⅰ型酮病与Ⅱ型酮病比较,获得24种血浆差异代谢物,主要为柠檬酸、组氨酸、β-葡萄糖、异亮氨酸、极低密度脂蛋白/低密度脂蛋白等,其中β-羟丁酸、低密度脂蛋白和极低密度脂蛋白、异亮氨酸、缬氨酸、丙酮、亮氨酸、乙酸浓度升高;柠檬酸、酪氨酸、组氨酸、肌醇、谷氨酰胺、β-葡萄糖、苯丙氨酸、谷氨酸、α-葡萄糖、赖氨酸、甲酸、甘氨酸、磷酸胆碱、丙氨酸、O-乙酰葡萄糖胺浓度呈现下降。【结论】1H NMR技术与多元统计分析的有效结合能够有效的筛选出Ⅰ型酮病、Ⅱ型酮病与健康对照组之间血浆差异性代谢物,为进一步探究奶牛Ⅰ型酮病、Ⅱ型酮病的发病机理和诊断与防治提供了新的方向。

Identification of Fucans from Four Species of Sea Cucumber by High Temperature ~1H NMR

Acidic polysaccharide, which has various biological activities, is one of the most important components of sea cucumber. In the present study, crude polysaccharide was extracted from four species of sea cucumber from three different geographical zones, Pearsonothuria graeffei(Pg) from Indo-Pacific, Holothuria vagabunda(Hv) from Norwegian Coast, Stichopus tremulu(St) from Western Indian Ocean, and Isostichopus badionotu(Ib) from Western Atlantic. The polysaccharide extract was separated and purified with a cellulose DEAE anion-exchange column to obtain corresponding sea cucumber fucans(SC-Fucs). The chemical property of these SC-Fucs, including molecular weight, monosaccharide composition and sulfate content, was determined. Their structure was compared simply with fourier infrared spectrum analyzer and identified with high temperature 1H nuclear magnetic resonance spectrum analyzer(NMR) and room temperature 13 C NMR. The results indicated that Fuc-Pg obtained from the torrid zone mainly contained 2,4-O-disulfated and non-sulfated fucose residue, whereas Fuc-Ib from the temperate zone contained non-, 2-O- and 2,4-O-disulfated fucose residue; Fuc-St from the frigid zone and Fuc-Hv from the torrid zone contained mainly non-sulfated fucose residue. The proton of SC-Fucs was better resolved via high temperature 1H NMR than via room temperature 1H NMR. The fingerprint of sea cucumber in different sea regions was established based on the index of anomer hydrogen signal in SC-Fucs. Further work will help to understand whether there exists a close relationship between the geographical area of sea cucumber and the sulfation pattern of SC-Fucs.

1H NMR对烟草甲虫蛀蚀款冬花前后化学成分的变化研究

目的:探究款冬花经烟草甲虫蛀蚀后化学成分的变化。方法:测定未虫蛀款冬花、烟草甲虫蛀蚀后的款冬花及烟草甲虫排泄物的氢核磁共振(^(1)H nuclear magnetic resonance,^(1)H NMR)图谱并进行化合物指认归属。采用主成分分析(principal component analysis,PCA)、偏最小二乘法-判别分析(partial least squares discriminate analysis,PLS-DA)和正交偏最小二乘法-判别分析(orthogonal partial least squares discriminate analysis,OPLS-DA)对虫蛀款冬花进行鉴别。根据变量重要性投影(variable importance in the projection,VIP)明确变化的化学成分,并采用t检验加以验证。结果:根据^(1)H NMR图谱共指认33个化合物。多元统计分析结果表明,未虫蛀款冬花、烟草甲虫蛀蚀后的款冬花和排泄物部分可分别聚为一类。从化学成分含量的差异结果看,款冬花被虫蛀后款冬酮的含量下降,在排泄物中异亮氨酸、缬氨酸等氨基酸的含量升高,绿原酸、异绿原酸等款冬花的次生代谢产物含量下降。结论:首次将^(1)H NMR结合多元统计分析用于中药材虫蛀后化学成分的变化研究,为中药材变质现象的研究提供了新的思路和方法。

Application of a quantitative ^1H NMR method for rapid extraction and determination of the content of paeonol in Cynanchum paniculatum

Cynanchum paniculatum(Bunge) Kitagawa is usually used as an herbal medicine for treating many diseases. Paeonol is the main active component, and its content is the key indicator for quality control of C. paniculatum. In the present study, we developed a rapid, accurate and precise method for quantitation of paeonol in C. paniculatum using 1 H NMR spectra. The deuterated solvent of methanol-d4 enabled satisfactory separation of the signals to be integrated in 1 H NMR spectrum. H-6(δ 7.78) of 1 H NMR spectrum of C. paniculatum was selected as the feature signal for quantitation, and trimesic acid(TMA) was selected as an internal standard. Validation of the quantitative method was performed in terms of linearity, specificity, repeatability and stability. This is the first time to report quantitative 1 H NMR(qHNMR) applied to determine the content of paeonol in C. paniculatum and showed a wider linearity range than the reported quantitation of paeonol in others. The simple extraction of paeonol from C. paniculatum was rapid and will prompt the application of the developed method. This work implied that qHNMR represented a feasible alternative to HPLC-based methods for quantitation of paeonol in C. paniculatum, and it was suitable for the quality control of C. paniculatum.

核桃壳木质素的^1H—NMR分析

在核桃壳磨木木质素(MW L)提取纯化的基础上,对纯化的核桃壳磨木木质素进行了C、H、O及OCH3含量的测定,并利用1H-NMR对核桃壳木质素基本化学结构进行研究。结果表明:(1)核桃壳木质素的C、H、O含量分别为67.15%、5.73%和27.12%,甲氧基含量为18.19%;(2)核桃壳木质素C9经验式为C9H9.22O1.99(OCH3)1.05,其C9单元结构的相对分子量为181.61;(3)核桃壳木质素属GS型木质素,其中G型木质素占多数,为80.68%;(4)核桃壳木质素中酚羟基(OHph)和脂肪族羟基(OHaliph)分别占总羟基数的32.21%和67.79%;(5)核桃壳木质素中存在较多的-βO-4、-β5和β-β结构。

基于~1H-NMR指纹图谱的四批市售桑白皮药材质量分析

目的采用核磁共振~1H-NMR指纹图谱技术,结合多元统计分析方法研究四种市售桑白皮药材与标准药材的化学成分差异性并评价其质量。方法以氘代甲醇-氘代重水(体积比1∶1)混合溶剂提取药材,在温度298 K,观测频率600.25 MHz条件下采集~1H-NMR谱,NMR数据经分段积分处理后,分别进行相似度分析、层序聚类分析和OPLS-DA分析。结果桑皮苷A、桑根皮醇、桑辛素、albanin A、grateloupinmaide、胆碱、蔗糖、乙酸、天门冬酰胺、葡萄糖、赖氨酸、氨基葡萄糖、精氨酸、丙氨酸、N-乙酰葡糖和柠檬酸是四种市售桑白皮药材与标准药材中有显著性差异的化学成分,桑皮苷A作为桑白皮的活性成分在四种市售药材中含量远低于标准药材,显示四种市售药材质量与标准药材存在较大差距。结论基于~1H-NMR和OPLS-DA的研究方法可以提供具体的差异性化学成分信息,并评价桑白皮药材的质量,为今后通过核磁共振技术建立桑白皮药材质量控制的方法提供参考和依据。

^(1)H NMR ERETIC2结合多变量分析法定量分析生麻黄与蜜炙麻黄差异

目的利用^(1)H NMR ERETIC2定量方法对14个批次的生麻黄和6个批次的蜜炙麻黄进行定性和定量分析,并筛选出差异成分,为麻黄质量标准的提升提供科学依据。方法以特征性成分麻黄碱信号强度为优选指标,对提取方法和复溶溶剂进行优化;建立基于^(1)H NMR ERETIC2方法的生麻黄和蜜炙麻黄特征成分绝对定量方法;采用^(1)H NMR谱图结合多变量分析法寻找不同批次生麻黄和蜜炙麻黄潜在的差异成分。结果最佳样品前处理方法为以甲醇为溶剂,物料比为1∶5(g/mL),超声提取5 min,氘代甲醇作为复溶溶剂。^(1)H NMR图谱共鉴定了11个化学成分,其中8个共有成分被选作定量指标。定量结果显示,生麻黄和蜜炙麻黄中异亮氨酸、蔗糖、葡萄糖和丙氨酸的含量差异有统计学意义(P<0.05);多元统计分析结果也表明,生麻黄和蜜炙麻黄之间存在明显差异,葡萄糖和蔗糖是主要的差异贡献成分,且在蜜炙麻黄中含量较高,而蜜炙麻黄中丙氨酸和异亮氨酸的含量则明显下降(P<0.05)。结论本研究建立的^(1)H NMR ERETIC2定量方法结合多元统计分析,可筛选出生麻黄和蜜炙麻黄的差异成分,能够有效区分生麻黄和蜜炙麻黄,为后续麻黄质量标准的完善提供了科学依据。

基于^(1)H-NMR技术的维生素E亚临床缺乏症 奶牛血清代谢谱分析

为了探究奶牛泌乳早期发生VE亚临床缺乏时体内代谢物的变化,在黑龙江省绥化市某规模化牛场随机选取背景信息(年龄、体况、胎次)相近的产后30 d内的高产奶牛,根据血浆中VE含量结合血液生化指标分为对照组(VE含量4μg·mL^(-1)以上)和VE亚临床缺乏组(VE含量2~3μg·mL^(-1)),每组14头,组内能量代谢、肝功、维生素含量、氧化应激等指标无差异,利用核磁共振氢谱(^(1)H-NMR)技术结合多元统计分析和生物信息学分析,获得VE亚临床缺乏奶牛血清差异代谢物。结果表明:与对照组相比,获得29种上调的差异表达代谢物,其中9种参与蛋白质的消化和吸收,10种参与氨基酸类物质代谢,10种参与糖类物质代谢及三羧酸循环(TCA)循环。差异代谢物主要参与氨酰基-tRNA合成,糖酵解或糖异生,丙氨酸、天冬氨酸与谷氨酸代谢,氮代谢及D-谷氨酰胺与D-谷氨酸代谢,与能量负平衡导致脂质分解代谢所致的氧化应激有关,也与VE亚临床缺乏促进能量负平衡和氧化应激有关。

基于^(1)H-NMR技术的慢性肾衰竭代偿期气阴两虚证血清代谢分析

目的分析基于^(1)H-NMR技术的慢性肾衰竭代偿期气阴两虚证的血清代谢情况。方法选择2019年1—11月山西省中西医结合医院肾三科收治的15例慢性肾衰竭代偿期气阴两虚证自愿患者作为疾病组,15例健康的病人家属及志愿者作为对照组。留取空腹静脉血并备样处理,利用^(1)H-NMR技术结合主成分分析(PCA)、正交偏最小二乘法判别分析(OPLS-DA)等多元化分析手段,寻找内生化合物并比较组间的代谢物差异变化。结果疾病组中精氨酸、脯氨酸、脂质等7种代谢差异物含量高于对照组,胆碱、磷脂酰胆碱2种含量低于对照组,差异均有统计学意义(P<0.05)。结论初步发现慢性肾衰竭代偿期气阴两虚证候学存在特定的代谢轮廓。CRF代偿期气阴两虚证的代谢紊乱途径可能主要涉及氨基酸及脂质代谢等方面。代谢组学技术可以更加全面的为中医肾脏疾病的现代化研究和临床实践提供有益的参考,为实现超早期诊疗慢性肾衰竭助力。

NMR-Metabolomic Study on Monocultivar and Blend Salento EVOOs including Some from Secular Olive Trees

The aim of the present work has been to characterize, by NMR-based metabolic profiling, extravirgin olive oils (EVOOs) from a subarea (Salento) of Apulia, leader EVOO producer among the Italian regions. According to the European Union (EU) definition, Protected Designation of Origin (PDO) products are mostly closely linked to the concept of terroir due to the place of origin, climate and local know-how. Moreover, the authenticity and traceability of several products such as olive oils with specific geographical origin require to be preserved by analytical methods. In this regard, about a hundred EVOO samples (monovarietal and blend samples, cultivars Ogliarola Salentina and Cellina di Nardò, basis of “Terra d’Otranto” PDO, campaign 2012-2013) were therefore analyzed by 1H NMR spectroscopy and multivariate statistical analysis. Both unsupervised (PCA) and supervised (OPLS-DA) statistical analyses allowed differentiation of monocultivar oils and blends characterization. Other features such as the age of the trees (young, 100 years) could also be investigated. Cellina samples showed a higher content of aldehydic and phenolic compounds, while Ogliarola samples were characterized by NMR signals in the range of δH 6.5 - 5.6, which could be ascribed to higher carotenoids content. Higher polyphenols and polyunsaturated fatty acid content were also found in young over secular tree EVOOs.

High-Resolution ¹H NMR Investigations of the Oxidative Consumption of Salivary Biomolecules by a Tooth-Whitening Formulation: Relevance to Safety Issues

A multicomponent evaluation of the oxidative consumption of salivary biomolecules by a hydrogen peroxide (H2O2)-containing tooth-whitening formulation has been performed using high-resolution proton (1H) nuclear magnetic resonance (NMR) spectroscopy. Unstimulated human saliva samples (n = 10) were treated with aliquots of supernatants derived from 1) the H2O2-containing whitening gel, 2) the corresponding tooth-whitening accelerant solution containing an amino-alcohol activator, and 3) a combination of these product agents pre-mixed in the recommended manner. 600 MHz 1H NMR spectra acquired on these samples demonstrated that H2O2 present in the whitening gel gave rise to the oxidative decarboxylation of salivary pyruvate (to acetate and CO2), the direct oxidation of trimethylamine and methionine (to trimethylamine-N-oxide and methionine sulphoxide respectively), and the indirect oxidative consumption of lactate and carbohydrates in general. Experiments conducted on a chemical model system confirmed the consumption of pyruvate by added H2O2, and also revealed that this method could be employed for determinations of the H2O2 content of tooth-whitening products. In conclusion, high-resolution 1H NMR analysis provides much valuable molecular information regarding the fate of tooth-whitening oxidants in human saliva, and also permits an assessment of the ability of endogenous antioxidants therein to protect against any soft tissue damage arising from the possible leakage of H2O2 from tooth-whitening application trays.

Determination of Meclofenoxate Content in Meclofenoxate Hydrochloride for Injection by DSC and 1H-NMR

Two simple and rapid analytical methods (DSC and 1H-NMR), are proposed for determination of meclofenoxate in meclofenoxate hydrochloride for injection. DSC thermogram is recorded without any sample pretreatment. The response linearity is ensured by linear determination factors R2, which is 0.9982. The recoveries of meclofenoxate hydrochloride in sterile powder for injection are from 98.3% to 102.3% (n = 3). The quantitative 1H-NMR is quick and simple to use. The quantitation of meclofenoxate is reproducible and the relative standard deviation is 1.0%. The accuracy of two methods is validated by comparison with the results obtained by HPLC. The results show that the two methods are capable of quantifying the content of meclofenoxate in meclofenoxate hydrochloride for injection.

^(1)H-NMR定量测定黄芪注射液中亲水性成分和疏水性成分

目的建立黄芪注射液中亲水性成分和疏水性成分的^(1)H-NMR定量分析方法。方法以10%氘代水(10%D2O)和氘代甲醇(CD3OD)为氘代溶剂制备黄芪注射液亲水性成分和疏水性成分的^(1)H-NMR样品。使用Bruker Avance Ⅲ 600型核磁共振波谱仪采集^(1)H-NMR图谱,具体实验参数如下:Noesygppr1D脉冲序列;温度为298 K,数据点32 K,采集时间(AQ)为2.980 s,脉冲宽度(SW)为7211.54 Hz,弛豫延迟时间(D1)分别为15.0 s和20.0 s,频率偏移(O1)分别为2816.65 Hz和2930.31 Hz,接收器增益(RG)值为57,扫描次数(NS)32次。结果在^(1)H-NMR图谱中归属出33种成分,分别是异亮氨酸、亮氨酸、缬氨酸、丙氨酸、乳酸、焦谷氨酸、天冬酰胺、γ-氨基丁酸、脯氨酸、甲酸、乙酸、富马酸、苹果酸、琥珀酸、丙二酸、蔗糖、果糖、半乳糖、葡萄糖、胆碱、甜菜碱、葫芦巴碱、尿苷、腺苷、胞苷、鸟苷、腺嘌呤、黄芪皂苷Ⅲ、黄芪甲苷、芒柄花苷、毛蕊异黄酮苷、9,10-二甲氧基紫檀烷-3-O-葡萄糖苷以及异黄烷苷。对其中27种化学成分(异亮氨酸、缬氨酸、丙氨酸、乳酸、焦谷氨酸、天冬酰胺、γ-氨基丁酸、脯氨酸、甲酸、乙酸、富马酸、苹果酸、琥珀酸、丙二酸、蔗糖、果糖、葡萄糖、胆碱、甜菜碱、葫芦巴碱、尿苷、腺苷、鸟苷、腺嘌呤、黄芪皂苷Ⅲ、黄芪甲苷、毛蕊异黄酮苷)进行定量,可定量的成分占注射液固含量90%以上。该方法的精密度、重复性、样品稳定性和耐用性良好,各个成分线性关系良好,r 2大于0.9990,加样回收回收率为98.19%~101.40%。结论建立了一种简单、快速、可靠的^(1)H-NMR定量方法用于测定黄芪注射液中的亲水性成分和疏水性成分,为黄芪注射液的质量评价提供了新的分析手段。

配位聚合物｛[Zn(CF_3COO)_2(C_5H_5ON)·]H_2O｝_n的合成、晶体结构及表征

new coordination polymer {[Zn(CF3COO)2(C5H5ON)]·H2O}n was synthesized based on the reaction of zinc(Ⅱ) trifluoroacetate and 3-hydroxypyridine(C5H5ON) in methanol medium for the first time. The structure of the coordination polymer was confirmed by IR, 1H NMR, elemental analysis and thermal analysis. The crystal structure of the coordination polymer was also determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group P21/m, and crystallographic data of the coordination polymer are: a= 0.863 1(4) nm, b=0.717 7(3) nm, c=1.116 4(5) nm, α=γ=90°, β=107.542(6)°, V=0.659 4(5) nm3; Dc=2.037 g·cm-3; Z=2; F(000)=400; μ=1.969 mm-1. Zinc(Ⅱ) atom lies at the center of an octahedron formed by the coordination of zinc atom and six O atoms which come from four different trifluoroacetate ions and two different 3-hydroxypyridine molecules where each trifluoroacetate ion and 3-hydroxypyridine are coordinated to two different zinc ions to form coordination polymer. CCDC: 253909.

应用光谱分析技术研究土壤水溶性有机质的分组及其结构特征

本研究以Leenheer的分组方法为基础 ,采用XAD 8树脂分组水稻土水溶性有机质 (DOM ) ,并通过元素组成、1H NMR和FTIR详细研究了疏水酸性 (HOA)、酸不溶 (AIM )、疏水中性 (HON)和亲水性 (HIM)等组分的结构特征。土壤DOM组成中HOB含量最少 ,HON含量为 7%～ 15 % ,HIM是土壤DOM中最大组成部分 ,达 35 %以上 ,HOA与AIM之和为 5 0 %左右。元素分析、FTIR及1H NMR分析结果表明DOM各组分结构特征差异显著 ,HON以含有大量的长链烷烃为主要结构特征 ,并含有较多氨基酸、多肽等含氮类物质。HOA类似于土壤富里酸 (FA) ,含有大量羧基 ,但与FA相比芳香族物质减少 ,碳水化合物增多。AIM以多酚类、腐殖质结合的碳水化合物为主要组成物质。

锌盐与二甲氧基嘧啶配合物的光谱研究

无水乙醇中回流制得ZnCl_2和ZnSO_4与2-氨基-4,6-二甲氧基嘧啶(AMP)的1:2和1:1固态配合物,用化学分析和元素分析确定它们的组成分别为Zn(AMP)_2Cl_2(A)和Zn(AMP)SO_4(B);用IR,XPS和~1HNMR研究了它们的成键情况。IR光谱分析说明配合物中,配体通过氨基N原子及嘧啶环上一个N原子与Zn^(2+)双齿配位,配合物B中SO_4^(2-)参与了配位;XPS谱证明配合物A中和B中SO_4^(2-)均参与了配位,并且N→Zn^(2+)键中有不同程度的反馈键;~1H NMR说明配合物A中有2个配体参与配位,配合物B中只有1个配体参与了配位。由此推测了它们的可能结构。

瓜环与喹啉衍生物包结配合行为研究

利用1H NMR以及荧光技术研究了六、七、八元瓜环与2-苯基喹啉、N-正丙基溴化异喹啉、3-氨基喹啉及7,8-苯并喹啉的相互作用.两种方法的考察结果均表明,2-苯基喹啉能与这3种瓜环发生相互作用,其中六、七元瓜环与2-苯基喹啉形成1∶1的稳定包结配合物,包结常数分别为1.6×104和3.2×103L/mol.八元瓜环能与2-苯基喹啉形成1∶2包结物.1H NMR结果还表明,3种瓜环均能与N-正丙基溴化异喹啉相互作用,其化学计量比均为1∶2;七元瓜环与7,8-苯并喹啉相互作用,化学计量比约为1∶1.荧光法也表明八元瓜环能与N-正丙基溴化异喹啉、3-氨基喹啉及7,8-苯并喹啉发生相互作用,并且荧光强度随瓜环浓度增加而下降,其化学计量比为1∶2.同时,讨论了上述主客体包结配合物的作用模式.

碳纳米管对苯酚和α-萘酚的吸附研究

研究了20℃时碳纳米管对苯酚和α-萘酚的吸附,测定了不同浓度下碳纳米管对它们的吸附量,并采用Langmuir方程进行拟合,根据1H质子宽线氢谱和热重分析对吸附结果进行了探讨。结果表明,碳纳米管对α-萘酚的吸附能力较对苯酚的吸附能力强,碳纳米管与α-萘酚之间存在较强的π-π共轭作用,而与苯酚之间的π-π共轭作用较弱。

μ-氧-双[三(对氟苄基)锡]的合成、表征及晶体结构

The μ-oxygen-bis[tri(p-fluorobenzyl)tin] was synthesized. The structure were characterized by elementary analysis, IR and 1H NMR and the crystal structure were determined by X-ray single crystal diffraction. The crystal of the title compound belongs to rhombohedral with space group R, a=1.346 4(4), b=1.346 4(4), c=1.772 9(7) nm, α=90°, β=90°, γ=120°, Z=3, V=2.783 2(15) nm3, Dc=1.625 g·cm-3, μ(Mo Kα)=1.408 mm-1, S=1.088, F(000)=1 350, R1=0.027 5, wR2=0.065 9. In compound, the tin atom has a distorted tetrahedral coordination configuration. CCDC: 257079.

升麻的^1H—NMR指纹图谱-模式识别研究

目的:建立一种基于1H-NMR指纹图谱-模式识别的不同品种升麻的鉴别方法。方法:以1H-NMR技术测定升麻中三萜皂苷类特征提取物的信息,并转化为数据矩阵,采用化学模式识别方法中的主成分分析(PCA)及判别偏最小二乘(DPLS)法进行识别分析。结果:1H-NMR指纹图谱-模式识别能够有效地鉴别不同品种的升麻样本。结论:1H-NMR指纹图谱-模式识别是一种有效的药材分类鉴别方法,可以作为药材质量控制的手段之一。