优化高效液相色谱法测定棉籽粕中游离棉酚的含量

本试验旨在建立一种测定棉籽粕中游离棉酚含量的高效液相色谱(hPLC)法的优化方法.试验采用丙酮提取棉籽粕样品,经超声、离心、抽滤、旋转蒸发处理,用乙腈-0.2％磷酸(体积比为85∶15)溶液溶解;色谱条件为:色谱柱Agilent TC-C18(250mm×4.6mm,5μm),流动相为乙腈-0.2％磷酸(体积比为85∶15)溶液,流速1.0mL/min,紫外检测波长235nm,进样量20μL,柱温25℃.结果得出,游离棉酚的回归标准曲线为y=189347x+24969(r=0.99999),在游离棉酚含量为0.1224～78.336 μg/mL范围内线性良好,最低定量限为0.52mg/kg;棉籽粕样品36h内4℃稳定性的相对标准偏差在1.51％～3.43％;平均回收率在94.72％～99.49％,相对标准偏差在1.72％～3.13％.可知,本方法稳定性好,准确度、灵敏度和回收率高.     

HPLC法测定盐酸氯苯胍原粉含量

目的：采用高效液相色谱法测定盐酸氯苯胍的含量。方法：样品经1％盐酸甲醇萃取．以SHIMADZUC8色谱柱（250mm×4．6mm,5μm）分离,甲醇和2．5％的磷酸溶液以体积比75比25的混合液为流动相,在检测波长为317nm处测定。结果：峰面积与盐酸氯苯胍的质量浓度在1—100．0mg·L^-1范围内呈线性关系。标准加入回收率为（n=6）95．2％,相对标准偏差（n=5）小于0．5％。     

油制磺胺间甲氧嘧啶钠混悬注射液HPLC含量测定方法的研究

建立了油制磺胺间甲氧嘧啶钠(SMM-Na)混悬注射液含量测定的HPLC方法。样品中加入表面活性剂使其成为微乳溶液,然后稀释进样分析。色谱柱为phenomenex synergi Hydro-RP(250 mm×4.6 mm,4μm),柱温40℃,以甲醇-乙腈-1.5%冰乙酸水溶液(10∶20∶70)为流动相,流速为1 mL/min,检测波长271 nm。同一样品经永停滴定法和HPLC两种方法进行含量测定并进行t检验分析,结果显示t0.05,P0.05,呈显著差异。HPLC测定制剂的平均含量为98.99%,RSD为0.48%。磺胺间甲氧嘧啶在20～60μg/mL的浓度范围内与峰面积呈良好的线形关系。本方法更简单、快速、准确,可用于油制磺胺间甲氧嘧啶钠混悬注射液的含量测定。     

RP-HPLC双波长法测定四味穿心莲散中穿心莲内酯和脱水穿心莲内酯的含量

建立了反向高效液相色谱法检测四味穿心莲散中穿心莲内酯和脱水穿心莲内酯含量的方法。试验采用十八烷基硅烷键合硅胶色谱柱(4.6 mm×250 mm,5μm),以甲醇-0.2%磷酸溶液梯度洗脱,流速为1.0 m L/min,柱温30℃;穿心莲内酯检测波长226 nm,脱水穿心莲内酯检测波长252 nm;穿心莲内酯和脱水穿心莲内酯的含量测定范围分别为2.32~37.14μg/m L(r=1.0000),2.00~31.94μg/m L(r=1.0000);加样平均回收率分别为99.12%、98.84%;RSD分别为0.60%、0.62%;该方法方便、准确、可靠,适用于测定四味穿心莲散中穿心莲内酯和脱水穿心莲内酯的含量。     

Effects of dietary fructo-oligosaccharide on villous height and disaccharidase activity of the small intestine,pH, VFA and ammonia concentrations in the large intestine of weaned pigs

Abstract

An experiment was conducted to investigate changes in the lumen and wall of the intestinal tract of weaned pigs caused by fructo-oligosaccharides (FOS) and consequences for growth. Twelve male pigs weaned at 24 days were individually housed and fed either control, 0.25% FOS, or 3% FOS diets for 21 days after weaning. The pH of chyme in the caecum and proximal colon were lower (p<0.001) in 3% FOS compared to other treatments. Mean molar proportions (%) of total SCFA values along the large intestine were significantly affected by FOS diet. Acetic acid was significantly higher in control compared with other treatments. Butyric acid and isobutyric acid were significantly increased in 0.25 and 3% FOS compared to the control. Feed intake, empty body weight gain, disaccharidase activities and villous height in the small intestine were not significantly affected by FOS. It was concluded that dietary FOS stimulates fermentation in the large intestine, but does not significantly affect enzyme activity, ammonia content, villous height and growth.     

固相萃取-高效液相色谱法测定乳制品中三氯蔗糖

建立乳制品中三氯蔗糖的固相萃取高效液相色谱检测方法.采用0.2％乙酸水溶液沉淀蛋白,提取三氯蔗糖,然后通过C18固相萃取柱进行净化浓缩后,采用高效液相色谱-蒸发光散射检测仪进行检测,该方法0.1～0.8g/L范围内以三氯蔗糖进样质量的对数和相应峰面积的对数做标准曲线,R2为0.9991,相关性良好,加标回收率在94％～102％之间,检出限为2.0mg/L(RSN=3).     

防己散质量控制方法研究

对《中国兽药典》2005年版防己散的质量标准进行修订,采用薄层色谱法对制剂中防己药材进行定性鉴别,采用高效液相色谱法对粉防己碱和防己诺林碱进行了含量测定。建立了同时测定防己散中2种成分含量的方法,粉防己碱和防己诺林碱的线性范围分别为52．55～525．5μg／ml（r=0．9995）和27．30～273．0μg／ml（r=0．9996）;平均回收率（n=9）分别为98．1％（RSD=1．9％）和97．9％（RSD=2．2％）。该方法简便、准确、重复性好,为防己散的质量控制提供了定量方法。     

Changes in growth performance, digestive enzyme activities and nutrient digestibility of cherry valley ducks in response to aflatoxin B1 levels

The objective of this study was to investigate toxic effects of aflatoxin B1(AFB₁) on growth performance, organs, hepatic enzyme activities, apparent digestibility of nutrients and digestive enzyme activities in ducks. Ninety 1-day-old Cherry Valley commercial ducks were designed to three treatment groups with three replicates of ten birds each. Group I (control) was fed conventional feed free of AFB₁, group II or III was fed the diets containing 20 μg/kg or 40 μg/kg AFB₁-contaminated rice respectively. The feeding trial lasted 6 weeks. The results were that decreased body weight gain and feed intake, increased feed to gain ratio and selected organ weights (liver, kidney and pancreas) were observed in AFB₁-treated groups. The activities of serum alanine aminotransferase (ALT) and aspartate aminotransferase (AST) were significantly increased in AFB₁-contamined groups. The apparent digestibility of crude protein (CP) was significantly lower while activities of digestive enzyme from duodenum contents including protease, chymotrypsin, trypsin and amylase were increased in AFB₁-treated group. These results indicated that AFB₁ of feed could decrease growth performance and apparent digestibility of nutrients, change digestive enzyme activities of duodenum contents in duck.     

猪鸡联养研究

研究表明笼养肉鸡的鸡粪中粗蛋白含量比平面养的高１６．４７个百分点，而粗纤维低９．１２个百分点。用鸡粪喂猪，其饲料报酬同加入鸡粪的比例呈正相关，如日粮中添加３０－６０％鸡粪，其饲料报酬提高１５．３２－５５．３２％；同样加入４０％鸡粪喂猪，鸡粪经发酵的饲料报酬又比不发酵的高９．６２％。为使育肥猪得到较好的增重，还应将日粮的营养水平调整到接近饲养标准，猪鸡联养规模，一个专业户一次批量以肉鸡１０００－１５００羽，联养生猪１０－２０头为宜。     

板蓝根注射液的HPLC特征图谱研究

目的：建立板蓝根注射液HPLC特征图谱。方法：色谱柱为Waters Atlantis T3(5μm,4.6×250mm),以甲醇为流动相A,以水为流动相B,进行梯度洗脱;流速为0.8ml/min;柱温为30℃;检测波长为250nm。结果：板蓝根注射液的色谱图基本相同,检出特征共有峰有9个。结论：该方法简便,灵敏度高,重复性好,结果准确可靠,可作为板蓝根注射液有效的鉴别和质量评价方法。