大米中有机磷和氨基甲酸酯农药残留检测方法研究

应用石英毛细管气相色谱法,利用高灵敏氮磷检测器,用乙腈和丙酮提取样品,建立了一种快速测定大米中有机磷和氨基甲酸酯8种农药残留的方法.结果表明,该方法的最低检出浓度为0.002～0.009 mg/kg.添加量为0.004～O.007mg/kg时,添加回收率为84.3%～120.0%,相对标准偏差为4.1%～11.5%.该方法能同时测定大米中的有机磷和氨基甲酸酯类农药,具有灵敏度高、分离效果好、回收率高、变异系数小、检出限低的特点.     

大豆种子脂肪氧化酶缺失基因控制豆腥味效果的研究

 应用蒸馏提取法、气相色谱和气 -质联机的方法分析了大豆种子脂肪氧化酶缺失体近等位基因系在加工豆制品时所产生的挥发性气味物质。研究结果表明 ,从豆粉和豆浆中都只分离出 2 4种气味成分 ,主要为醛和醇类物质 ;在形成挥发性气味物质和豆腥味物质中 L ox2起主要作用 ,L ox1次之 ,L ox3作用最小 ,但具有降低己醛生成的作用 ;不论缺失 L ox1,还是缺失 L ox2 ,都可极显著地降低挥发性气味物质和豆腥味物质的生成量 ,而缺失 L ox3则会显著增加己醛的生成量 ;缺失基因间存在有显著或极显著的一级和二级负互作 ;不同加工条件对缺失基因的缺失平均效应和互作效应有明显的影响。全缺失体类型具有最低的挥发性物质和豆腥味物质的生成量 ,而缺 L ox3类型具有最高的生成量 ,其余的缺失体类型则介于两者之间 ;用己醛作为衡量脂肪氧化酶在形成豆腥味中的重要性和各种缺失体类型控制豆腥味效果的指标是可行的。因此 ,培育出大豆种子脂肪氧化酶全缺失的品种将有望成为食品加工业的优质原材料     

高效液相色谱法测定更乐霉素残留量试验

蛋鸡饲料中添加GRC50×10~(-6),300×10~(-6),600×10~(-6),连续喂4个月。600×10~(-6)组蛋品中残留GRC6×10~(-6),其它组无残留;伊沙公鸡饮水中添加GRC2.5g/L,连续饮用86d,休药3d测定。肌肉、肝、脾、肾、心GRC残留量分别为0.0369×10~(-6)。0.0449×10~(-6),0.031×10~(-6),0.0296×10~(-6),0.029×10~(-6),0.5 g/L,1g/L组无残留;明显肉鸡饲料中添加GRC600×10~(-6),连续喂36d,休药2d测定,肌肉、肝、脾、肾、心GRC残留量分别为0.0432×10~(-6),0.0478×10~(-6),0.0342×10~(-6),0.0524×10~(-6),0.0432×10~(-6),50×10~(-6),300×10~(-6)组无残留;肉猪饲料中添加GRC 600×10~(-6),连续喂115d,休药5d测定,肌肉、肝中GRC残留量分别0.0318×10~(-6),0.0056×10~(-6)。50×10~(-6),300×10~(-6)组无残留。     

模拟移动床色谱分离玉米须粗提物

在无标样的情况下,应用模拟移动床色谱分离玉米须粗提物,并得到含量为92%的产品。经液质、红外、紫外鉴定为黄酮类。     

Urinary free metanephrines measurement in dogs with adrenal gland diseases using a new simple liquid chromatography tandem mass spectrometry method

Measurement of urinary metanephrines in spot samples is used for the diagnosis of canine pheochromocytoma (PC). We describe a simple analytical method based on liquid chromatography tandem mass spectrometry (LC-MS/MS) for measuring free metanephrine (MN) and normetanephrine (NMN) in spot urine samples. Using the developed method, we evaluated the stability of urinary free-MN and free-NMN at various storing conditions. In addition, we assessed the feasibility of urinary free-MN and -NMN measurement for diagnosing PC. Urine samples were mixed with stable isotope internal standards and thereafter purified by ultrafiltration. The purified samples were analyzed by LC-MS/MS in the multiple reaction monitoring mode after separation on a multimode octa decyl silyl column. The coefficient of variation of free-MN and -NMN measurement was 7.6% and 5.5%, respectively. The linearity range was 0.5–10 µg/l for both analytes. Degradation was less than 10% for both analytes under any of the storage conditions. The median free-NMN ratio to creatinine of 9 PC dogs (595, range 144–47,961) was significantly higher (P<0.05) than that of 13 dogs with hypercortisolism (125, range 52–224) or 15 healthy dogs (85, range 50–117). The developed method is simple and may not require acidification of spot urine. The results of this preliminary retrospective study suggest that the measurement of urinary free metanephrines is a promising tool for diagnosing canine PC.     

Estimation of genetic parameters for carcass grading traits,image analysis traits,and monounsaturated fatty acids in Japanese Black cattle from Hyogo Prefecture

Genetic parameters for carcass grading traits, image analysis traits, and monounsaturated fatty acid (MUFA) percentages were estimated in 29,942 Japanese Black cattle from Hyogo Prefecture. The analyzed traits included five carcass grading traits, two image analysis traits, fat area ratio and fineness index, and two MUFA traits, one measured in intermuscular fat using near-infrared spectroscopy (NIRS) and the other in intramuscular fat using gas chromatography (GC). The heritability estimates of image analysis traits and MUFA were moderate to high, ranging from 0.395 to 0.740, and it was considered that they could be improved simultaneously with carcass grading traits because no severe genetic antagonism was observed. Although the heritability of the NIRS-based intermuscular MUFA was slightly lower than that of the GC-based intramuscular MUFA, the genetic correlation between the two methods was as high as 0.804. These results indicate that the NIRS method can be used as an alternative evaluation procedure to predict MUFA in intramuscular fat in the longissimus muscle.     

穿心莲内酯超临界CO2重结晶工艺初探

采用单因素实验法探讨超临界CO₂重结晶压力、温度、时间对穿心莲内酯的纯度和结晶率的影响，并借助扫描电镜进行晶体形貌考察，利用高效液相色谱仪进行纯度检测。结果表明，采用超临界CO₂重结晶技术得到的穿心莲内酯晶体形貌更加细小，并呈絮状分布在结晶板上；选择较佳纯化工艺参数为重结晶压力14 MPa，温度55℃，时间60 min，CO₂流量20 L/min时，得到的穿心莲内酯纯度达90%以上，结晶率超过45%。     

Determination of neutral sugars in soil by capillary gas chromatography after derivatization to aldononitrile acetates

We have quantified ribose, rhamnose, arabinose, xylose, fucose, mannose, glucose, and galactose in soil by gas chromatography (GC) simultaneously after converting to aldononitrile acetate derivatives. A recommended single-hydrolytic step by 4 M trifluoroacetic acid (TFA) at 105 °C for 4 h was more effective for releasing soil neutral sugars from non-cellulosic carbohydrates and better suited to our purification procedure compared with the sulphuric acid hydrolysis. Linearity of the GC detection for each neutral sugar was in the range of 10-640 μg ml⁻¹ and the recovery of neutral sugars from the spiked soil samples ranged from 76% to 109.7%. The coefficients of variation of the neutral sugars in four soils were lower than 2.0% for the instrument and 4.6-7.6% for the whole determination procedures. Compared with the trimethylsilyl (TMS) derivatization, the recovery of our newly modified method was more satisfactory and the reproducibility of ribose was improved significantly. Moreover, the aldononitrile acetate derivative was more stable than TMS derivative. Therefore, it is a promising approach suitable for a routine use in the quantitative analysis of soil neutral sugars, since it is fast, sensitive, and reproducible.     

Amino-N compounds found in soil organic matter hydrolysates of a loamy sand using an immobilized protease reactor column

Summary Soil organic matter (OM) from seven different fertility plots of a loamy sand was extracted and fractionated into high- and low-molecular-weight (HMW, LMW) fractions using gel filtration. The fractions were acid-hydrolyzed to determine the amino sugar and amino acid contents. The same fractions were hydrolyzed with an immobilized protease reactor column. Reverse-phase high-performance liquid chromatography (HPLC) was used to identify the soil amino-N compounds. With the HMW fraction as substrate, the enzyme released less than 1% of 11 amino-N compounds determined by acid hydrolysis. Phenylalanine and leucine, however, were recovered in quantities of 2% and 4%, respectively. Immobilized protease hydrolysis of the LMW fraction recovered considerably more amino-N compounds compared with acid hydrolysis of the same fractions. Each system of hydrolysis produced some amino-N compounds not found in the other. We conclude that an immobilized enzyme reactor column will allow a researcher to perform time-course hydrolysis, so that hydrolysis intermediates, e.g. peptides, can be separated and identified.     

藏系绵羊乳酸脱氢酶A的分离纯化和酶学性质

采用HiTrapTM Blue HP亲和层析和DEAE-Sephadex离子交换层析分离方法，对1只雄性高原藏系绵羊(Ovis aries) 大腿骨骼肌乳酸脱氢酶-A(LDH-A)进行了分离纯化，并对其酶学参数进行了测定。纯化的藏系绵羊乳酸脱氢酶-A比活力为100.94 U/mg蛋白，纯化倍数为 12.0。经PAGE和SDS-PAGE分析均显示1条带。酶动力学参数测定显示：Km(米氏常数)NADH(reduced nicotinamide adenine denucleotide)=0.022，Km丙酮酸钠=0.444，均比家兔的高；丙酮酸还原反应的最适pH约为5.8；草酸和二价汞能抑制LDH-A的活力；二价汞是LDH-A的可逆性抑制剂。