国产克洛素隆尿药排泄数据分析

应用Kromasil-C18色谱柱(250 mm×4.6 mm,5 μm),WatersTM480型可调波长紫外检测器,0.01M磷酸钾(pH=7):乙腈(3:1)为流动相,检测波长265 nm,含量测定采用标准曲线法,建立了RP-HPLC法检测绵羊尿中克洛素隆含量的方法.方法有效性评价结果表明,尿药含量在0.01～5.0μg/ml及5.0～30.0μg/ml范围呈良好线形关系(r=0.9993、0.9995),方法平均回收率99.32%,日内、日间变异系数分别为3.91%、6.28%.尿药最低检测限0.005μg/ml.试验绵羊以7 mg/kg单剂量经静脉、肌肉及口服三种途径给药后,尿中药物浓度分析表明,克洛素隆经体内处理后主要经肾脏排泄,给药96 h内,静注经尿排泄原药为81.76%,肌注为64.03%,口服为48.50%.     

敌百虫的液相色谱分析方法

本文采用即以乙腈+水(50+50)为流动相,用CN柱和紫外检测器分离测定敌百虫原药及40%敌·毒乳油中敌百虫反相高效液相色谱法。结果表明,本方法的标准偏差为0.3233,变异系数为0.3551%,平均回收率为99.65%,线性相关系数为0.9997。     

Glu-B1位点亚基色谱鉴定及7OE对面团强度的影响

准准确鉴定高分子量谷蛋白亚基（HMW-GS）及探讨其对面团特性的影响是小麦品质研究的重要内容。用聚丙烯酰胺凝胶电泳（SDS-PAGE）和反相高效液相色谱（RP-HPLC）对62份品种（系）的HMW-GS组成进行鉴定。结果表明，结合SDS-PAGE和RP-HPLC两种方法可以对Glu-B1位点，尤其是Glu-B1（7+8）进行有效鉴定。选用13份姊妹系为材料，使用RP-HPLC和凝胶色谱（SE-HPLC）方法，研究了Glu-B1al（7^OE+8*）以及贮藏蛋白组分含量对面团强度的影响。结果表明，Glu-B1al（7^OE+8*）可显著提高HWM-GS总量和面团强度，7OE可作为优质亚基用于强筋小麦育种。相关性分析表明，谷蛋白总量、HWM-GS、LMW-GS以及x-HMW含量与最大抗阻力呈1%显著正相关，相关系数分别为0.76、0.76、0.77和0.72。SDS-不溶性谷蛋白大聚体（UPP）占谷蛋白聚合体总量的百分比与揉面仪峰值时间、粉质仪形成时间和稳定时间以及最大抗阻呈1%或0.1%显著正相关，相关系数分别为0.77、0.90、0.89和0.87。醇溶蛋白与谷蛋白含量的比值与揉面仪峰值时间呈1%显著负相关，相关系数为－0.69；与粉质仪稳定时间和最大抗阻呈5%显著负相关，相关系数分别为－0.58和－0.64。HPLC可有效分离和量化HWM-GS，并作为小麦品质育种有效的辅助手段。     

Polymerisation of gluten proteins in developing wheat grain as affected by desiccation

The breadmaking quality of wheat is affected by the composition of gluten proteins and the polymerisation of subunits that are synthesised and accumulated in developing wheat grain. The biological mechanisms and time course of these events during grain development are documented, but not widely confirmed. Therefore, the aim of this study was to monitor the accumulation of gluten protein subunits and the size distribution of protein aggregates during grain development. The effect of desiccation on the polymerisation of gluten proteins and the functional properties of gluten were also studied. The results showed that the size of glutenin polymers remained consistently low until yellow ripeness (YR), while it increased during grain desiccation after YR. Hence, this polymerisation process was presumed to be initiated by desiccation. A similar polymerisation event was also observed when premature grains were dried artificially. The composition of gluten proteins, the ratios of glutenin to gliadin and high molecular weight-glutenin subunits to low molecular weight-glutenin subunits, in premature grain after artificial desiccation showed close association with the size of glutenin polymers in artificially dried grain. Functional properties of gluten in these samples were also associated with polymer size after artificial desiccation.     

反相HPLC法快速测定鸭蛋蛋黄粉中胆固醇含量

通过RP-HPLC方法，比较了不同的流动相、流速、检测波长和温度对鸭蛋蛋黄粉中胆固醇分离效果的影响。确定试验最佳条件为：流动相：乙睛：甲醇：异丙醇＝50∶80∶10(体积比)，柱温45℃，进样量20 μL，流速1.3 mL/min，检测波长205 nm。在此条件下测得的天然红心鸭蛋蛋黄粉和普通鸭蛋蛋黄粉中胆固醇的含量分别为24.84 mg/g和25.75 mg/g。     

RP-HPLC法测定杜仲叶发酵液中绿原酸的含量

建立反相高效液相色谱(HPLC)法测定杜仲叶发酵液中绿原酸的含量。色谱条柱SymmetrySheildRP18柱(3.9mm×300mm,5μm),以水-甲醇-乙酸(88∶12∶1.2,V/V)为流动相,流速1.0ml/min,检测波长326nm,柱温25℃。绿原酸对照品在2.24～11.2μg范围内线性关系良好(r=0.9993)。该方法简便、准确、线性范围宽,可用于含绿原酸的原料及产品的质量控制。     

An expeditious HPLC method to distinguish Aconitum kusnezoffii from related species

An optimized HPLC-DAD method aided by similarity and hierarchical clustering analysis (HCA) was applied for identification of four species of the roots of Aconitum. The unique properties of this HPLC fingerprints and HCA were validated by analyzing Aconitum kusnezoffii Rchb. (AKR) samples and related herbs including A. karacolicum Rapcs. (AKP) samples, A. austroyunnanense W.T.Wang (AAW) samples and A. contortum Finet & Gagnepain (ACF). The results revealed that the chromatographic fingerprint combining similarity measurement and hierarchical cluster analysis could efficiently identify and distinguish AKR samples from its related species.     

赤水河下游水产品中辛基酚和壬基酚的测定

建立了固相萃取-反相高效液相色谱法测定水产品中辛基酚和壬基酚残留量的检测方法。样品经三氯乙酸溶液提取,阴离子交换固相萃取柱净化。色谱柱为Shim-pack VP-ODS 250 mm×4.6 mm,检测波长为225 nm,流动相为甲醇-水(体积比为75∶25),流速为0.8 mL/min,进样量为20μL。辛基酚和壬基酚分别在0.13～97.92μg/mL(R2=0.996 1)、0.02～50.00μg/mL(R2=0.999 4)浓度范围内与峰面积成良好线性关系,辛基酚和壬基酚的回收率为87.4%～93.7%,相对标准偏差为1.3%～3.9%。该方法准确、快速、灵敏度高,适用于水产品中辛基酚和壬基酚的检测。     

丹参抗氧化成分及其分布特征

借助超声波萃取法，以反相高效液相色谱（RP－HPLC－DAD）为分析检测手段，研究了丹参6种抗氧化成分的提取方法和分离定量条件，并对这些成分在全株丹参不同部位中的含量分布特征进行了探讨，结果表明：常温下的超声波萃取可避免热解作用给丹参酮类化合物带来的损失，布辅助的加热处理可使原儿茶醛获得较高的提取率，两种操作方法简单可行，6种化学成分在丹参不同部位及不同等级中的分布有较大差异，丹参酮类化合物主要分布在根部皮层，而叶子中丹参素的含量却较为丰富，可为丹参品质鉴定和质量标准研究及该资源的综合利用奠定理想基础。