LC-MS/MS测定猪尿中的黄曲霉毒素M1

建立LC-MS/MS检测猪尿中黄曲霉毒素M1的含量。猪尿样用超纯水稀释定容,充分漩涡振荡后经免疫亲和层析柱净化,甲醇洗脱,微孔滤膜过滤,经液相色谱分离,电喷雾离子源离子化,多反应离子监测(MRM)方式检测。外标法定量。采用0.1%甲酸:乙腈+甲醇溶液(1+1)为流动相,梯度洗脱。0.3mL/min的流速。在0.01μg/kg～0.50μg/kg范围内具有良好的线性关系,最低检测限为0.01μg/kg,回收率在70%～95%之间。此法操作简便、快速、灵敏、准确、样品处理简便易行,适用于测定猪尿中的黄曲霉毒素M1。     

Study on the Stability of Sheep Oxytocin in the Osmotic Pump

The experiment was aimed to evaluate the stability of oxytocin in osmotic pump (ALZET^®) at 39.1℃. The experiment was divided into 3 groups, i.e. the osmotic pump group, microcentrifugal tube group and control group. The control group remained frozen at -80℃, the other two groups were incubated in 39.1℃ incubator, and the samples were collected at different time points. All samples were analyzed by ultra-performance liquid chromatography tandem quadrupole/flight time mass spectrometry (UPLC-Q-TOF MS) method. The oxidation process of oxytocin in osmotic pump at 39.1℃ was analyzed by comparing the peak area of main oxidized products extracted ion chromatogram. The results showed that the degree of oxidation increased with time in osmotic pump and microcentrifugal tube at 39.1℃, and there was no significant difference between the two groups (P >0.05). The percentage of oxytocin prototype of samples which collected at different time points of osmotic pump group and microcentrifugal tube group versus control group were 83.6% to 117.8% and 83.2% to 116.2%, respectively, suggested that the trials involved in the osmotic pump implantation of oxytocin in sheep need to consider the effect of content changes caused by oxytocin oxidation on the test results.     

Performance assessment of nanoparticulate lime to accelerate the downward movement of calcium in acid soil

Calcium in conventional lime (CL) moves downward extremely slowly into the soil in the short term. To monitor the effects of using nanoparticulate lime (NL) in low affordable doses and in large doses on accelerating the downward movement of Ca in a simulated plough layer profile (0–25 cm), we ran a column leaching experiment with an acid soil with NL applied into the top 5 cm. The experiment evaluated a reference treatment (0 NL), three low doses of NL (8, 40 and 80 kg ha^?1 = 0.02×, 0.1×, and 0.2× the NL needed to raise soil pH to 6.0 in the top 5 cm: NLR_pH‐6), and two large doses (400 and 800 kg ha^?1 = 1× and 2× NLR_pH‐6). Over the short term (70 days), NL accelerated the downward movement of Ca, likely by mass flow of nanoparticles down soil micro‐ and macropores. Applying NL to the top 5 cm at 40 and 80 kg ha^?1 was effective at increasing the downward movement of Ca and the neutralization of soil acidity (in terms of pH) to 20 cm depth, as well as rectifying Al toxicity (in terms of exchangeable Al) to ≤ the critical limit to 10 cm. NL at 80 kg ha^?1 was most economically justified in terms of rectifying Al toxicity throughout the profile. Therefore, NL may introduce new and alternative application strategy that allowing lower rates of lime to be used and thereby offset economic constraints posed by high application rates.     

离子色谱法测定烤烟中氯离子和硫酸根离子及氟离子

提出了用离子色谱法测定烤烟中氯离子和硫酸根离子及氟离子的方法．采用IonPacASl4A阴离子交换分离柱、8mmol／L碳酸钠和1mmol／L碳酸氢钠混合液为流动相,自动再生抑制型电导检测在15min内完成烤烟中F^-1,Cl^-1,SO4^2-的测定,建立起针对烤烟F^-1,Cl^-1,SO4^2-的离子色谱法分析方法．该法具有良好的线性（相关系数为0．9991～0．9999）和重复性（相对偏差小于4．31％）,回收率为95．2％～103．1％．     

黄硬皮马勃萃取物柱层析馏分杀虫活性研究

[目的]研究黄硬皮马勃萃取物柱层析馏分的杀虫活性。[方法]对黄硬皮马勃总浸膏石油醚萃取物进行柱层析分离。经过梯度洗脱以及等体积收集,选择Rf值相同的收集液进行合并、减压浓缩,并对不同的馏分进行杀虫活性测定。[结果]黄硬皮马勃萃取物柱层析馏分对粘虫3龄幼虫均表现出一定的拒食活性;黄硬皮马勃二级柱层析馏分B2对粘虫3龄幼虫具有较强的触杀活性。[结论]可望开发出基于馏分B2的新杀虫剂产品。     

玉米中氯虫苯甲酰胺残留的超高效液相

研究建立了快速检测玉米中氯虫苯甲酰胺残留的超高效液相色谱(UPLC)分析方法。样品用乙腈-二氯甲烷[V(乙腈)∶V(二氯甲烷)=20∶80]提取,经N-丙基乙二胺(PSA)分散固相萃取剂净化,UPLC分离,二极管阵列检测器于254 nm处检测,外标法定量。结果表明:当添加水平为0.02~1 mg/kg时,平均回收率为81% ~91%,相对标准偏差(RSD)为6.2% ~14.0%;最小检出量(LOD)为 0.02 ng,最低检测浓度(LOQ)为0.02 mg/kg。方法的灵敏度、准确度及精密度均符合农药残留分析要求,适用于玉米中氯虫苯甲酰胺的残留分析。     

超声波辅助3种溶剂分析测定杜仲胶含量

杜仲生产的反式-1,4-聚异戊二烯橡胶(杜仲胶)是由异戊二烯单元聚合形成的不同分子大小的混合物,主要沉积于细胞的空隙之间,提取困难。为正确分析测定杜仲材料中杜仲胶的含量,以杜仲果翅为材料,采用氯仿、石油醚和甲苯3种有机溶剂,配合超声波处理组成6种不同的提取方法,以杜仲胶的提取得率以及分子量分布为衡量标准,对杜仲胶的分析测定方法进行比较。结果表明,采用氯仿作为有机溶剂,杜仲胶提取得率明显高于其他方法,可达到7.47%;氯仿配合超声波处理,会更进一步促进小分子或大分子杜仲胶聚合物的溶出和提取,所得杜仲胶的分子量分布范围更宽,分子量分布指数可达9.99。     

超声辅助-漂浮固化分散液液微萃取-气相色谱法测定茶叶中5种拟除虫菊酯类农药残留

建立了超声辅助-漂浮固化分散液液微萃取(UA-DLLME-SFO)-气相色谱法(GC)测定茶叶中甲氰菊酯、氟氯氰菊酯、氯氟氰菊酯、氰戊菊酯、溴氰菊酯5种拟除虫菊酯类农药残留的方法。获得最佳试验条件为20μL十六烷(萃取剂)和800μL丙酮(分散剂),质量分数为4%的氯化钠,水相pH为4,35℃超声30 min,-3℃、10 000 r·min~(-1)离心5 min后,去除水相后经气相色谱测定。结果表明:在1~150μg·kg~(-1)范围内,5种拟除虫菊酯类农药呈良好的线性关系,相关系数均大于0.9994,在1~5μg·kg~(-1)添加水平下,平均回收率为92.3%~99.6%,日内相对标准偏差(RSD)均低于3.5%(n=6),日间相对标准偏差(RSD)均低于5.9%(n=3),5种农药在茶叶中的检出限为0.11~0.24μg·kg~(-1),定量限为0.36~0.81μg·kg~(-1)。该方法操作简便、快速、安全、成本低、重现性好,适用于茶叶样品中拟除虫菊酯类农药残留的分析。     

气相色谱法测定稻米中毒死蜱的不确定度

对用气相色谱法测定稻米中毒死蜱农药残留的不确定度进行了评定。通过对测定过程中各变量的分析,确定了不确定度的来源,建立了相关数学模型,并对各变量的不确定度进行计算,最终算出合成不确定度。当水稻中的毒死蜱农药残留量为0.107 mg/kg时,测定结果的扩展不确定度为0.013 mg/kg(k=2)。     

超高效液相色谱法测定啶酰菌胺和咯菌腈在番茄与土壤中的残留

应用超高效液相色谱仪建立一种同时检测番茄和土壤中啶酰菌胺和咯菌腈残留的分析方法。样品经乙腈提取,乙二胺-N-丙基硅烷（PSA）吸附净化,以乙腈和水为流动相等度洗脱,采用可变波长紫外检测器检测,外标法定量分析。结果表明,啶酰菌胺和咯菌腈在0.05~1 μg/mL范围内呈现良好的线性关系,相关系数R ²均为0.999,方法的检出限均为0.01 mg/kg,定量限为0.1 mg/kg;在0.1~1 mg/kg范围内,添加回收率在82.8%~102.8%和86.5%~115.3%之间,相对标准偏差（RSD）在4.1%~8.7%和4.9%~9.1%之间。该方法简单可靠、重现性好,适用于番茄和土壤中啶酰菌胺和咯菌腈的残留检测。