RP-HPLC测定木槟硝黄散中木香烃内酯、去氢木香内酯的含量

建立了RP-HPLC法测定木槟硝黄散中木香烃内酯与去氢木香内酯含量的方法。用十八烷基键合硅胶柱分离木槟硝黄散中木香烃内酯与去氢木香内酯,以甲醇-水(60∶40)为流动相,检测波长225 nm。木槟硝黄散中木香烃内酯与去氢木香内酯的线性范围分别为4.14~41.4μg/m L和3.59~35.9μg/m L,平均回收率分别为99.23%、99.00%(n=6)。该方法简便、快速,可用于木槟硝黄散中木香烃内酯与去氢木香内酯的含量测定。     

盐酸塞拉嗪对大鼠不同脑区Gln及AsP含量的影响

研究盐酸塞拉嗪麻醉下大鼠不同脑区兴奋性氨基酸类神经递质含量的变化,探讨盐酸塞拉嗪中枢麻醉作用的可能机理.将48只Wistar大鼠随机分成6组,分别为对照组、诱导组、麻醉组、恢复Ⅰ组、恢复Ⅱ组和恢复Ⅲ组.采用反向高效液相色谱法测定各脑区Glu和Asp的含量.结果表明:腹腔注射盐酸塞拉嗪40 mg·kg-1后,麻醉组大鼠海马和丘脑Glu、Asp的含量显著降低(P＜0.05或P＜0.01),而小脑和大脑皮质Glu、Asp的含量显著增加(P＜0.01);恢复Ⅰ组除脑干外其它各脑区Glu和Asp的含量与对照组比较差异显著(P＜0.05);恢复Ⅱ组各脑区Glu和Asp的含量均恢复显著(P＞0.05);麻醉全程,脑干内Glu和Asp含量均无显著变化(P＞0.05).结果提示,盐酸塞拉嗪对海马、丘脑、小脑和大脑皮质内Glu、Asp含量的影响可能是其产生全麻作用的重要机理之一.盐酸塞拉嗪的中枢麻醉作用,可能与降低海马和丘脑内Glu、Asp,增加小脑和大脑皮质内Glu、Asp的含量有关,海马可能是盐酸塞拉嗪作用的最敏感的脑区.     

恩诺沙星及其代谢产物在中华绒螯蟹血淋巴中的比较药代动力学

研究了不同水温(16℃、25℃)、不同给药剂量(10 mg/kg、20 mg/kg)和不同给药方式(肌注、口灌)等条件下,恩诺沙星及其代谢产物环丙沙星在中华绒螯蟹体内的药代动力学,比较了不同条件下药物在蟹血淋巴中的吸收、分布和代谢的差异。结果表明,恩诺沙星在蟹血淋巴中的药-时数据符合开放式二室模型。16℃时以10 mg/kg剂量肌注给药后,恩诺沙星在蟹血淋巴的主要药代动力学参数为:AUC96.818 mg/(L.h),Cmax6.54μg/mL,t1/2α0.851 h,t1/2β95.415 h;25℃时以10 mg/kg剂量肌注给药后,恩诺沙星的主要药代动力学参数为:AUC168.457 mg/(L.h),Cmax7.12μg/mL,t1/2α0.58h,t1/2β88.833 h;25℃时以20 mg/kg剂量肌注给药后,恩诺沙星的主要药代动力学参数为:AUC155.612 mg/(L.h),Cmax11.045μg/mL,t1/2α5.239h,t1/2β88.378 h;25℃时以10 mg/kg剂量口灌给药后,恩诺沙星的主要药代动力学参数为:AUC86.525 mg/(L.h),Cmax3.469μg/mL,t1/2α8.071h,t1/2β61.842 h。不同条件下,恩诺沙星在蟹血淋巴中的主要药代动力学参数差异较大。恩诺沙星的活性代谢产物环丙沙星在各种给药条件下的蟹血淋巴中均能检出,但含量均处于较低值,且药-时数据不能用房室模型拟合,表明恩诺沙星在蟹体内只有极少部分代谢为环丙沙星。     

The use of reversed-phase high performance liquid chromatography as an aid to the identification of European barley cultivars

Summary A reversed-phase high performance liquid chromatography (RP-HPLC) system was used to separate the storage proteins (hordeins) extracted from European barley cultivars. From a total of 38 barleys tested, 26 types of hordein patterns could be distinguished after RP-HPLC. This appears to be a marked improvement in resolution over that achieved in a similar survey of European barley cultivars using SDS polyacrylamide electrophoresis (32 hordein patterns resolved by SDS PAGE from a total of 160 spring and winter barleys tested).Different hordein patterns were resolved by RP-HPLC within each of two groups of barley previously classified by SDS PAGE as indistinguishable within groups (three distinct patterns identified in a total of five cultivars tested from group 1A and five patterns observed among eight cultivars from group 3B). Thus RP-HPLC achieves a higher resolution than undirectional electrophoresis and promises to be a valuable aid in the identification of European barley cultivars.     

RP—HPLC法同时测定白头翁汤中盐酸小檗碱、盐酸药根碱、盐酸巴马汀的含量

目的：建立反向高效液相色谱方法同时测定白头翁汤中盐酸小檗碱、盐酸药根碱、盐酸巴马汀的含量。方法：色谱柱为XPODS—AC。。（250minx4．6mm,5I．Lm）;采用线性梯度洗脱方法,流动相：溶液A为乙腈,溶液B为O．05mol／L磷酸二氢钾（磷酸调pH值至3．0）。0—40min溶液A：溶液B为5：95—45：55;流速：1．0mL／min;柱温：室温;检测器：DAD检测器;检测波长：340nm;进样量：10μL。结果：盐酸小檗碱、盐酸药根碱和盐酸巴马汀分别在62．5-l000μg／mL、46．875—750μg／mL和37．5—600μg／mL范围内线性良好;平均加样回收率分别为99．22％（RSD为3．25％）、98．46％（RSD为1．99％）和99．20％（RSD为1．69％）。结论：本方法简便、灵敏、准确,适用于白头翁汤的质量控制。     

反相高效液相色谱同时测定菊花中黄芩苷和木犀草素的含量

建立一种同时测定黄芩苷和木犀草素的高效液相色谱检测方法,并分析菊花中黄芩苷和木犀草素的含量。样品采用超声提取,以0.1%磷酸溶液（A相）-甲醇（B相）为流动相,梯度洗脱程序：0-3 min,30%A～35%A;3-6 min,35%A～40%A;6-9 min,40%A;流速为1.0 mL/min;采用purospher star RP-18（250 mm×4.6 mm,5μm）色谱柱分离;检测波长327 nm;进样量20μL。黄芩苷和木犀草素分别在4.30-43.00 mg/L、5.00-50.00 mg/L范围内线性关系良好（r〉0.999 5）。加标回收率分别为100.2%和98.56%;相对标准偏差为3.2%和1.7%。该方法简便、快速、准确,适用于菊花中黄酮类化合物黄芩苷和木犀草素的检测和含量测定。     

盐酸环丙沙星在患子宫内膜炎奶牛子宫内给药的药物浓度

本研究以反相高效液相色谱为定量分析手段，选用5头患子宫内膜炎的奶牛，通过子宫内灌注盐酸环丙沙星（2.5 g/头），研究了盐酸环丙沙星在患子宫内膜炎奶牛体内的药物动力学规律。以二氟沙星为内标，血浆样品经甲醇沉淀蛋白，离心，经针头式过滤器处理，用反相高效液相法测定其中盐酸环丙沙星的浓度。 色谱条件为：ODS-1C₁₈柱；测定流动相为0.015 mol/L四丁基溴化铵溶液-乙腈（92∶8，V/V），pH为3.0；流速为1.0 ml/min；荧光检测器，激发波长（λex）278 nm，发射波长（λem）465 nm。通过采用MCPKP房室分析程序，分析血中浓度 时间数据，发现有3头奶牛血样药时数据符合无吸收三室开放模型。其血样中主要药动学参数为：T_1/2α为0.916 h、T_1/2β为49.20 h、AUC高达7.6296 mg/L·h、Clβ为1.582 L/kg·h，β为0.642 h^-1。有2头奶牛血样药时数据符合一级吸收二室开放模型。其主要药动学参数为：T_1/2α为1.26 h、T_1/2β为9.2 h、AUC高达28.336 mg/L·h，β为0.3571 h^-1。试验结果表明，盐酸环丙沙星子宫给药吸收快，分布广，消除慢。     

高纯度茄尼醇的分离及测定

探讨以烟叶浸膏为原料,经醇碱溶液皂化,采用乙醇水溶液和石油醚混合溶液萃取皂化物中的茄尼醇,再以甲醇分离茄尼醇,并经层析柱纯化,制备高纯度茄尼醇;以反相高效液相色谱法(RP-HPLC)测定样品中茄尼醇含量,流动相为乙腈∶异丙醇=7∶3,检测波长为210 nm,流速为1.0 m l/m in,柱温为室温,测定结果是样品中茄尼醇含量达98.51%,平均加样回收率为98.35%,标准偏差为1.75%。     

Characterization of two 1D-encoded ω-gliadin subunits closely related to dough strength and pan bread-making quality in common wheat (Triticum aestivum L.)

Gliadin proteins of 113 common or bread wheat (Triticum aestivum L.) cultivars and advanced lines from China and other countries, were analyzed by high performance capillary electrophoresis (HPCE) and reversed-phase high performance liquid chromatography (RP-HPLC). A major protein peak migrating at 3 min by HPCE and eluting at about 20 min by RP-HPLC was identified in the ω-gliadin region. It was present in cultivars with good pan bread-making quality, whereas most cultivars with poor bread-making quality lacked this protein peak. Quality testing and statistical analysis showed that this ω-gliadin peak was significantly related to dough strength, loaf volume and loaf score. It was separated into two apparent protein components by one-dimensional SDS-PAGE and two-dimensional electrophoresis (2-DE). According to their relative mobilities on the gels, the proteins were designated ω-15 and ω-16, and their accurate molecular masses (42590.5 Da for ω-15 and 41684.1 Da for ω-16) were determined by MALDI-TOF-MS. The ω-15 and ω-16 gliadins possessed the N-terminal amino acid sequences of ARELNPSNKELQQQQ and KELQSPQQQF, and therefore they belonged to 1D-encoded ω-2 type and ω-1 type gliadins, respectively. Both gliadin subunits were always present together among the 86 cultivars analyzed, suggesting that they were encoded by two closely linked genes at Gli-D1 locus. The accumulative characteristics of gliadins during grain development indicated possible additive quantitative effects of ω-15+16 on dough strength. The ω-15 and ω-16 gliadins could be used as valuable genetic markers for wheat quality improvement.     

RP-HPLC法测定2种银杏外种皮中黄酮苷含量

采用RP-HPLC法测定2种银杏主栽品种佛指和洞庭黄外种皮中黄酮苷含量.方法为:采用Shim-Pack VP-ODSC18(150mm×4.6mm,5 μm),流动相为甲醇:0.4%磷酸溶液(50:50),检测波长为360nm;流速为1 mL/min,柱温为30℃,以槲皮素、山柰酚和异鼠李素为对照外标法定量检测.试验结果表明,佛指和洞庭黄外种皮中黄酮苷含量分别为0.134%和0.150%,它们外种皮中黄酮苷含量不同,其中佛指中黄酮苷含量较高.