高效液相色谱法分析砂糖桔中嘧菌酯残留

采用配备有Hypersil ODS C18(250 mm×4.6 mm,5μm)色谱柱和紫外检测器的反相高效液相色谱仪,测定砂糖桔中嘧菌酯残留。以乙酸乙酯/环己烷(V/V=1/1)为提取溶剂,超声波提取砂糖桔中的嘧菌酯,经固相萃取净化,采用液相色谱法测定残留量。确定砂糖桔中嘧菌酯的最佳液相色谱检测条件为:检测波长257 nm,流动相V(乙腈)/V(水)=70/30,流速1.0 mL/min,进样量10μL。嘧菌酯在样品中的添加回收率为85.23%~92.04%,最低检测浓度为0.01μg/g,能满足农药残留分析要求。     

Characterization of core collection of lentil germplasm for phenology, morphology, seed and straw yields

Increasing and maintaining crop residues in predominantly cereal-based rotations of the US Pacific Northwest is critical to controlling soil erosion. The core collection of lentil (Lens culinaris Medik.) germplasm comprising 287 accessions was evaluated for variation in phenological, morphological and growth parameters including seed yields and residue amounts over a two-year period under conventional tillage and no-till conditions. The objectives of this study were (i) assess lentil genetic variation in germplasm for variation in biomass production and seed yield, (ii) assess the relationship of phenological and morphological traits with biomass and seed yield and (iii) identify high biomass producing germplasm for use as parents in the breeding program. Days to flowering and days to maturity ranged from 31 to 78 and from 71 to 106 days, respectively. Time to flowering in terms of cumulative heat units was a more efficient measurement than days to flowering. Plant height and plant canopy width had a significant association with total biomass, seed yield and residue amounts. Total biomass ranged from 788–6389 kg ha^–1 under conventional tillage, while the range under no-till conditions was 1045–6195 kg ha^–1. Most of the lines with higher biomass also produced the highest seed yields and residue amounts. Overall, only one accession produced more residue than `Laird'. In the more favorable environment of 1997, six accessions exceeded the control cultivars, `Laird' and `Indianhead', for residue amounts, and seven and twenty-four accessions exceeded control cultivars, `Pardina' and `Brewer', for seed yield. Results indicated that plant height, canopy width at maturity and seed yield explained most of the variation in biomass and residue production. Large seeded germplasm consistently had a longer reproductive growth period than small seeded accessions and had 17%, 7% and 21% more biomass, seed yield and residue, respectively. Our data indicated significant variation in lentil germplasm for biomass, seed yield and residue amounts to warrant their use in the breeding program.     

家禽肌肉组织中硝基咪唑类药物残留高效液相色谱检测法研究

 建立了检测家禽肌肉组织中甲硝唑、洛硝哒唑、二甲硝咪唑残留的高效液相色谱法。样品经乙酸乙酯振荡提取 ,浓缩 ,盐酸溶解残渣 ,己烷萃取除去脂肪。氢氧化钠调节溶液到pH 4 .8～ 5 .2 ,过C18小柱 ,甲醇洗脱 ,SpherisorbC18柱分离 ,32 0nm处检测。流动相为醋酸缓冲液 乙腈 (85∶15 ,v/v)。甲硝唑、洛硝哒唑和二甲硝咪唑检测限分别为 0 .5、1.0和 1.0ng·g-1。肉鸡肌肉组织中添加 6 .0ng·g-1水平回收率分别为 :甲硝唑 89.8% ,洛硝哒唑81.7% ,二甲硝咪唑 86 .6 %。此方法具有定性合理 ,检测限低 ,分析快速 ,准确等特点。     

不同栽培介质中铅、镉在茭白产品中残留的差异

[目的]为茭白的卫生安全生产提供参考依据。[方法]以单季茭品种"蒋墅茭"和双季茭品种"葑红早"为试材,以苇末和土壤为栽培基质进行不同浓度Cd2+、Pb2+胁迫处理,测定不同采收标准的产品器官中Cd2+、Pb2+残留量的变化。[结果]茭白产品器官对Cd2+、Pb2+的最高生物富集系数分别为0.340%和0.044%。过老发绿的肉质茎中,Cd2+、Pb2+的残留量最高,中等大小的肉质茎中残留量最低,且随重金属胁迫浓度的增加而显著增加。苇末基质栽培的茭白肉质茎中Cd2+、Pb2+的残留量均显著低于土壤栽培的。"葑红早"产品器官中Cd2+的残留量高于"蒋墅茭",Pb2+的残留量则相反。[结论]苇末栽培基质有利于降低重金属离子在茭白产品中的残留量。     

市售小麦和玉米中矮壮素残留现状调查

[目的]了解市售小麦和玉米中矮壮素的残留现状。[方法]建立了高效液相色谱-串联质谱分析小麦和玉米中的矮壮素的方法,并对产自4个不同省份的玉米和小麦样品进行了抽样检测。[结果]小麦和玉米样品经甲醇超声提取、高效液相色谱-串联质谱测定,小麦中矮壮素添加浓度分别为0.5～10.0 mg/kg时,平均回收率达96%～103%,变异系数为2.6%～4.3%,玉米中矮壮素添加浓度为0.5～10.0 mg/kg时,平均回收率达92%～98%,变异系数为2.0%～3.7%,最低检出浓度(LOQ)为0.01 mg/kg,方法的准确度、精密度、灵敏度均符合农药残留的分析要求;所测4个省份玉米和小麦样品中矮壮素的残留量水平均低于方法的最低检出浓度(0.01mg/kg)。[结论]为市场小麦和玉米中矮壮素残留监管提供了参考。     

液相色谱-串联质谱法测定牛奶中11种光引发剂残留量

建立了牛奶中11种光引发剂残留的定性和定量测定分析方法。样品经Carrez试剂沉淀蛋白质后,使用乙腈提取,HLB固相萃取柱净化,乙腈洗脱,洗脱液用氮气吹干后用50%乙腈水溶液定容,采用液相色谱-串联质谱进行测定。分析物采用电喷雾电离,正离子扫描,多反应监测(MRM)模式检测,其中7种光引发剂使用内标法定量,4种光引发剂使用外标法定量。11种光引发剂在5.00～200μg/L浓度范围内线性关系良好,相关系数均大于0.990。11种光引发剂的测定低限均为1.0μg/kg。在添加浓度1.00～100μg/kg范围内,加标回收率为74.3%～112%,相对标准偏差为0.57%～16.3%。本方法简便、有效、灵敏,适用于牛奶中光引发剂多残留的定量测定和确证。     

酶联免疫吸附法在磺胺类药物残留检测中的应用

介绍了磺胺类药物的毒性及其残留量的检测方法,着重叙述了酶联免疫吸附法及其在磺胺类药物残留检测中的应用。     

Changes in mineral nitrogen, phosphorus availability and salt-extractable aluminium following the application of green manure residues in two weathered soils of South Vietnam

Phosphorus deficiency and aluminium toxicity in weathered soils can be amended by applying organic residues. Nitrogen mineralization, changes in P-availability and changes in salt-extractable Al following the incorporation of residues of various green manures (Flemingia congesta, Mucuna pruriens, Pueraria phaseoloides, Tithonia diversifolia) were quantified in a field core incubation experiment. Dried residues were added at an application rate of 45 kg P ha⁻¹ to two soils representative for the main soil groups of the South Vietnamese uplands, set up in incubation cores in an experimental field near Ho Chi Minh City, Vietnam.Decomposition of the residues proceeded at high rates. Mineralized nitrogen from the residues was recovered mainly as ammonium during the first 2 weeks of incubation. Nitrogen release from Tithonia residues with the highest lignin content and lignin:N ratio occurred more gradually compared to the three legumes. Resin-extractable P was significantly increased by residue treatments. Largest and sustained increases in resin-extractable P (0.67 and 2.06 mg P kg⁻¹ in the two soils) were observed in samples amended with Tithonia, which was related to the large P-content (0.37%) and small C:P ratio (110) of the residues. The P-concentration in the residues, rather than the total amount of P applied through the residues, affected the increase in P-availability. The increase in resin-extractable P was correlated to the P-content (R=0.64) and C:P ratio (R=−0.65) of the residues. Salt-extractable Al-concentrations were considerably reduced by the organic amendments, up to 70 and 50% in the two soils. At the rate of 45 kg P ha⁻¹, no significant differences between the residue treatments to reduce soil acidity were observed.As such, the application of high quality residues that are rich in P, in particular T. diversifolia, may enhance crop production by creating favourable soil conditions during the initial stages of plant development of the main crop.     

青霉素菌渣残留降解物的蓄积毒性研究（摘要）（英文）

[目的]初步研究青霉素菌渣残留降解物的蓄积毒性,进而探讨其是否具备作为蛋白饲料投入养殖业开发利用的条件。[方法]通过小鼠亚急性毒性试验,饲喂小鼠不同剂量的青霉素菌渣降解物（3%和6%）连续观察15周,记录每周小白鼠的体重和死亡情况;试验结束后抽样处死,取血测动物肝、肾功能,取心、肝、脾、肾称重,并在光镜下对肝、肾组织做病理学观察。[结果]试验组小白鼠体重、死亡率及肝、肾功能在15周内和对照组差异均不显著（P〉0.05）。低剂量组可见肝细胞、肾小管上皮细胞核有碎裂,少数肝、肾细胞有轻度水肿;高剂量组可见小白鼠肝组织中细胞核碎裂并有脂肪滴,多数肝细胞水肿,只有少数肝细胞无明显改变;肾脏可见门管区炎性细胞浸润,肾小管上皮细胞水肿、坏死。[结论]该实验条件下青霉素菌渣降解物对小鼠器官的实质细胞有轻度的毒性作用。     

阿灭净在菠萝与土壤中的残留及消解动态研究

采用气相色谱(GC-NPD)分析技术测定除草剂阿灭净在菠萝与土壤中的残留及消解动态结果表明,GC-NPD方法的最小检出量为0.0232ng,菠萝及土壤的最小检出浓度分别为0.002mg/kg和0.005mg/kg,GC-NPD方法回收率分别为87.23%~92.10%和88.80%~93.77%。喷施阿灭净80%WP4800g(a.i/)hm2,处理检测出菠萝与土壤中原始沉积量分别为0.1448~0.1646mg/kg和3.3318~3.5536mg/kg,消解半衰期分别为29.17~29.45d和25.75~30.68d,按阿灭净用量4800g(a.i/)hm2施药菠萝1次,间隔期为10d,菠萝果实残留量2年分别为0.1646mg/kg和0.1448mg/kg,参照欧共体的MRL值0.2mg/kg,按上述阿灭净剂量方法施用菠萝是安全的。