QuEChERS耦合UPLC-MS/MS同时测定葡萄中9种植物生长调节剂

目的:采用液质联用同时测定葡萄中α-萘乙酸、多效唑、2、4-D、矮壮素、吲哚-3-丁酸、6-苄基腺嘌呤、氯吡脲、缩节胺和对氯苯氧乙酸9种植物生长调节剂。方法:样品按Qu ECh ERS方法前处理采用乙腈提取、PSA净化,以乙腈-10 mmol/L乙酸铵(0.05%氨水)溶液为流动相,梯度洗脱,Waters ACQUITY UPLCTMBEH C18(2.1 mm×100 mm,1.7μm)不锈钢色谱柱分离,三重四级杆质谱多反应监测方式检测,外标法定量。结果:9种植物生长调节剂在线性范围内具有良好的线性关系,线性相关性r≥0.99,检出限在0.15~8.89μg/kg,加标回收率在77.2%~112.0%,相对标准偏差在2.08%~9.12%。结论:该方法耗时短、操作简单、有机试剂使用少,灵敏度高、回收率好,适用于日常葡萄中多种植物生长调节剂检测,可缩短检测周期。     

PET瓶中UV-P和UV-234两种光稳定剂的迁移研究

建立了PET瓶中2种光稳定剂2-(2'-羟基-5'-甲基苯基)苯并三唑(UV-P)和2-(2-羟基-3',5'-二枯基苯基)-苯并三唑(UV-234)的高效液相色谱检测方法。两种光稳定剂在质量浓度为0.5μg/m L~20μg/m L的范围内线性良好,相关系数R0.99,加标浓度为2、4、10μg/m L的加标回收率为76.2%~111.7%,相对标准偏差为1.2%~11.7%,UV-P和UV-234的检出限分别为0.05μg/m L和0.07μg/m L,并用该方法对市售食品的PET瓶进行了检测。最后根据欧盟法规使用50%(v/v)和95%(v/v)的乙醇以及异辛烷作为食品模拟物对PET样品瓶中2种光稳定剂的迁移进行了研究。     

HPLC法测定乳饮料中纽甜含量的研究

建立快速、准确测定乳饮料中纽甜含量的高效液相色谱检测方法。样品以20%乙腈水溶液为提取液,硫酸锌和亚铁氰化钾为沉淀剂进行前处理,采用ZORBAX SB-C18(250 mm×4.6 mm,5μm)色谱柱,200 nm检测波长,磷酸氢二铵(0.020 mol/L,pH 3.5~4):乙腈=(70∶30)为流动相进行等度洗脱分离。纽甜在0.2μg/m L~50.0μg/m L范围内线性良好,在0.8 mg/kg~5.0 mg/kg加标范围内,回收率为90.1%~96.1%,RSD值为1.7%~2.1%,最低定量限为0.30 mg/kg。     

亲水作用色谱-电喷雾串联质谱法测定水产品中的氟苯尼考胺的残留量

建立亲水作用色谱-电喷雾串联质谱测定水产品中氟苯尼考胺残留量的测定方法。样品用碱性乙酸乙酯提取,以正己烷和脂肪吸附材料去除油脂,用5 mmol/L乙酸铵溶液(含0.2%甲酸)和乙腈作为流动相,以梯度洗脱方式在Acquity UPLC BEH HILIC柱(55 mm×2.1 mm,1.7μm)色谱柱上分离,以电喷雾离子源正离子模式进行质谱分析,基质外标法定量。结果表明,氟苯尼考胺的质量浓度在0.1~20μg/L范围内呈良好的线性,相关系数(r2)大于0.990。在1.0~50.0μg/kg加标水平下,虾、黄鱼、鳗鱼、烤鳗的平均回收率为70.5%~87.7%,相对标准偏差为4.8%~11.6%,定量限为1.0μg/kg。该方法简单、灵敏、稳定,可满足水产品中氟苯尼考胺残留量的检测和确证需要。     

凝胶渗透色谱-高效液相色谱法测定植物油中苯并芘

建立了用凝胶渗透色谱-高效液相色谱法测定植物油中苯并芘的方法。该方法以乙酸乙酯-环己烷(1:1,v/v)提取样品,凝胶渗透色谱净化,以ZORBAXSB-C18柱(4.6mm×250mm,5μm)分离,流动相为甲醇和水(90+10),流速1.0mL/min,激发波长365nm,发射波长412nm,柱温25℃,进样量25μL。该方法的检出限0.4μg/kg,线性范围0.1~10.0μg/L,加标回收率98.7%~109.2%,相对标准偏差为3.81%~8.76%。     

离子交换固相萃取-超高效液相色谱-串联质谱法快速测定腐竹中的乌洛托品

目的建立腐竹中乌洛托品的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。方法样品经乙腈/水(1:1,v:v)溶液超声提取,阳离子交换柱净化后,经Waters Acquity UPLC BEH HILIC(2.1 mm×100 mm,1.7μm)色谱柱分离,在电喷雾正离子多反应监测模式下进行测定。结果乌洛托品在0.5~100.0μg/L范围内线性关系良好,相关系数(r)大于0.999。方法检出限和定量限分别为6μg/kg和20μg/kg。在20、40、100μg/kg 3个空白加标水平下,乌洛托品的加标回收率为100.1%~103.9%,相对标准偏差为4.7%~8.9%。结论该方法快速、简便、准确可靠,适用于腐竹中非法添加的乌洛托品的含量测定。     

反相高效液相色谱测定饮料中新橙皮苷二氢查尔酮

建立了反相高效液相色谱检测饮料中新橙皮苷二氢查尔酮的分析方法。分别对提取方法、沉淀剂的使用和色谱条件进行了优化。采用核壳型的Accucore C18(2.6μm,4.6 mm×100 mm)色谱柱为分析柱,以甲醇和水(45∶55,v/v)为流动相,等度洗脱,流速1.0 m L/min,柱温25℃,紫外检测波长283 nm,进样量10μL,外标法定量分析。结果表明新橙皮苷二氢查尔酮的分离在10 min以内,具有良好峰形,在0.5~50 mg/L浓度范围内,有良好的线性关系,相关系数r0.999,检出限为0.15 mg/L,在10、40、80 mg/kg加标水平下平均回收率在90.2%~103.5%之间,相对标准偏差(RSD)在1.96%~7.59%之间(n=6)。结果表明该方法选择性强、灵敏度高、操作简便,可用于饮料中新橙皮苷二氢查尔酮的检测。     

固相萃取-反相高效液相色谱法测定大黄鱼皮肤主要色素

借助固相萃取技术,利用反相高效液相色谱法定性和定量测定了大黄鱼皮肤主要色素。样品经丙酮和石油醚(v/v=4∶3)提取,加Na OH-甲醇溶液皂化反应后,经LC-NH2固相萃取小柱净化,洗脱剂为乙腈-甲苯(v/v=3∶1),液相色谱柱为ZORBAXEclipse XDB-C18柱(150mm×4.6mm,5μm),流动相为乙腈-甲醇(v/v=9∶1),流速1.0m L/min,采用二极管阵列检测器检测,检测波长为474nm,外标法定量。结果显示:大黄鱼皮肤主要色素为叶黄素,占比为50%以上,并含有少量的角黄素、虾青素及其他色素;且各色素线性关系良好,相关系数分别为0.9990、0.9991和0.9991,加标回收率分别为84.26%~96.56%、83.28%~92.79%和85.61%~94.39%,相对标准偏差分别为2.55%~5.78%、3.52%~7.28%和3.02%~6.55%,检出限分别为0.43、0.59、0.82mg/kg。     

液相色谱质谱法测定食品中咪唑菌酮残留量

建立采用高效液相色谱串联质谱仪测定植物源食品中咪唑菌酮残留量的分析方法。样品经丙酮提取,固相萃取活性炭柱净化,C18色谱柱分离,以乙腈和5 mmol/L乙酸铵甲醇水(v∶v=40∶60)溶液为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应选择离子监测(MRM)。结果表明:咪唑菌酮在0.05μg/m L~0.8μg/m L范围内呈现良好的线性关系,相关系数(r2)大于0.999。在此范围内加标回收率为80.08%~108.53%,相对标准偏差(RSD)为1.16%~6.03%,检测限为1.0μg/kg。该方法可以满足植物源食品中咪唑菌酮残留量监测的需求。     

超高效液相色谱-串联质谱法同时检测功能 食品中6 种玛咖酰胺

目的建立功能性食品中6种玛咖酰胺类物质的超高效液相色谱-串联质谱同时分析方法。方法样品经乙醚提取,氮气吹干,乙腈定容,Acquity UPLC BEH C_(18)(2.1 mm×100 mm,1.7μm)色谱柱分离,在正离子模式下以电喷雾电离多反应监测模式进行定性和定量分析。结果本方法在15 min内完成6种目标化合物的分离分析。6种玛咖酰胺在0.1~2μg/L范围内线性相关系数r0.999,6种玛咖酰胺检出限均为0.2μg/kg;各玛咖酰胺在3个浓度水平的加标回收率在74.5%~87.2%之间,相对标准偏差(relative standard deviation,RSD)在2.6%~6.3%之间(n=6)。结论该方法准确、可靠,适用于功能性食品中玛咖酰胺的检测。     

棉籽饼的脱毒与利用

在畜禽饲料中棉籽饼用量过大，棉酚含量超过畜禽的耐爱量，会引起畜禽中毒，饲喂前对绵籽饼进行物理法，化学法或生物法脱毒均可达到较好的脱毒效果。对于棉籽饼作猪，牛，鲤鱼饲料的配合使用方法，试验情况和结果进行了介绍。无腺体棉籽中不含或有少量棉酚，用于饲养畜禽不会引起中毒，是一种新的蛋白质饲料资源。     

棉籽及棉籽油中苯并芘的来源研究

为了探究棉籽及棉籽油中的苯并芘来源,采用高效液相色谱法对不同来源地的棉籽进行了苯并芘含量测定,并对苯并芘含量较高的棉籽及不同含量苯并芘的棉籽制取的油脂进行了苯并芘含量分析。结果表明:一般棉籽中的苯并芘含量都不高且与种植区域无关,基本都小于1μg/kg;棉籽本身苯并芘含量不会增加,但在运输储存过程中会受到苯并芘污染,比如运输车辆打扫不干净,储存中受空气污染及尘土侵袭都有可能使棉籽中苯并芘含量升高;受污染的棉籽中苯并芘主要分布在棉籽壳上,棉籽中的苯并芘会在棉籽油中聚集。     

一种新的棉籽脱酚生产工艺

介绍了分步提油和萃取棉酚的工业化生产工艺,解决了工业化生产过程中遇到的设备和工艺问题.采用本工艺生产的脱酚棉籽粕中游离棉酚含量小于0.045%、残油小于1.5%、蛋白含量大于50%.     

利用有腺体棉籽粕生产食用棉仁分离蛋白的实践

棉仁蛋白是一种潜在的重要食品资源,由于棉酚的存在一直未被人类充分利用。通过甲醇脱酚、4#溶剂脱脂、低温连续脱溶的棉籽粕生产工艺和碱溶酸沉的蛋白生产工艺,于2001年首次实现了工业化利用有腺体棉籽粕生产食用棉仁分离蛋白的实践,获得了高安全性的棉仁分离蛋白。     

The effects of varying gossypol intake from whole cottonseed and cottonseed meal on lactation and blood parameters in lactating dairy cows

Effects of varying amounts of gossypol from whole Upland cottonseed (WCS) and cottonseed meal (CSM) were evaluated in 40 midlactation Holstein cows. After 14 d of pretreatment, cows were assigned to 1 of the 5 treatments for 84 d: control (no gossypol), 931 mg/kg total gossypol (TG) and 850 mg/kg free gossypol (FG) from WCS (moderate TG and high FG); 924 mg/kg TG and 91 mg/kg FG from CSM (moderate TG and low FG), 945 mg/kg TG and 479 mg/kg FG with equal amounts of TG from WCS and CSM (moderate TG and FG), or 1894 mg/kg TG and 960 mg/kg FG with equal amounts of TG from WCS and CSM (high TG and FG). Concentrations of plasma gossypol (PG) and its isomers were directly proportional to FG intake. Concentrations of PG reached a plateau after 28 d on treatment, and they were highest in cows receiving a diet with high TG and FG. Erythrocyte fragility differed among treatments and increased with increasing FG intake. Plasma gossypol returned to negligible concentrations 28 d after withdrawal of cottonseed products from the high TG and FG diet. Serum vitamin A was similar among treatments, but vitamin E increased with increasing FG intake. Serum enzymes were generally unaffected by treatments, but urea N increased in diets higher in TG and FG. Intake of dry matter was higher for the diet high in TG and FG than for the control diet, but was similar for other treatments. Cows receiving the high TG and FG diet produced more milk and 3.5% fat-corrected milk, with no changes in milk composition. Feeding a diet containing 1894 mg/kg TG and 960 mg/kg FG for 84 d increased PG concentrations and erythrocyte fragility and resulted in minor changes in blood metabolites and enzymes, but no detrimental effect on lactation performance was observed. Indicators of liver, kidney, and muscle cell viability suggest that the higher amounts of gossypol consumed in this study had only minor effects on those tissues in lactating dairy cows.     

溶剂法浸出棉籽油和脱除棉酚的工艺研究

综述了采用单一溶剂或混合溶剂浸出棉仁生坯（或饼）,提取棉籽油并脱除棉籽粕中棉酚的工艺研究进展情况。     

Effects of source of gossypol and supplemental iron on plasma gossypol in Holstein steers

Four experiments were conducted to evaluate factors influencing concentrations of plasma total gossypol (TG) in 30 Holstein steers fed cottonseed products. At the end of each 28-d experiment, steers were weighed and blood samples were collected and analyzed for plasma TG concentrations. During the entire study, steers did not show any overt signs of gossypol toxicity. In the 28 d before experiment 1, 30 steers with a body weight (BW) of 273 kg were fed a standardization diet with 15.0% Upland whole cottonseed (WCS) that resulted in a mean intake of 9.08 g/d of TG per steer/d and a plasma TG of 1.66 μg/mL. In experiment 1, 30 steers were fed 1 of 5 diets with 15.0% Upland WCS, but different levels of supplemental Fe [0, 150, 300, 450, and 600 mg/kg of diet dry matter (DM)]. Average daily gain was not affected by level of Fe in the diet, but DM intake, plasma TG, and plasma TG response decreased linearly as Fe in diets increased. In experiment 2, steers were fed diets with 15.0% Upland cottonseed as whole, cracked, roasted, cracked-roasted, or extruded. Analysis of the seed revealed that roasting or extrusion markedly reduced free gossypol (FG) content. Minor effects on animal performance were observed, but plasma TG decreased with roasting or extrusion of seeds, with the greatest reduction when the seed was cracked and then roasted. In experiment 3, steers were fed 2 levels of WCS (7.0 or 14.0% of DM) with 3 levels of cottonseed meal (2.8, 5.5, or 8.5% of DM) in the diet. Animal performance was not altered by diet, but plasma gossypol concentrations and responses were greater in steers fed diets with more WCS, because of the greater FG intake. In experiment 4, 24 steers were fed diets with 15.0% cottonseed (Upland or Pima) either as whole or cracked. Pima cottonseed increased TG and FG intakes, which resulted in greater plasma TG concentration and response. Animal response to processing of cottonseed tended to differ according to type of cottonseed. However, feeding Pima and cracking of cottonseed increased gossypol availability and plasma TG concentrations.     

几株真菌对棉籽粕和棉籽壳脱毒的影响

以棉籽壳和棉籽粕为主要原料,利用酵母（JM-1、JM-2、JM-干1、JM-干2）、霉菌（MM-1、MM-2、MM-3、MM-4）,通过发酵试验确定最佳的脱毒菌种。结果表明,以JM-1效果最好。在棉籽粕中,JM-1能将棉籽粕中棉酚的含量由发酵前的0．2018％降低到0．0266％,MM-1能使棉籽粕的棉酚含量降低到0．...     

低酚棉籽蛋白及酶水解物乳化容量的研究

本项研究建立了低酚棉籽蛋白乳化容量的测定模型,并探讨了蛋白酶水解作用对两类低酚棉籽蛋白的影响。在10,000r/min的高度搅拌下,向低酚棉籽蛋白的食盐溶液中不断添加油脂,所形成的乳浊液的导电率逐渐下降并最终突跃降至零。在观察到导电率突跃降至零时立即停止加油。按照此方法对不同量的蛋白质分别测定其耗油量,发现耗油量与蛋白质量的线性相关,回归系数的值即为低酚棉籽蛋白质的乳化容量。可溶于水的低酚棉籽非贮存蛋白经酶水解后乳化容量呈下降趋势。随着水解程度的提高,不溶于水的低酚棉籽贮存蛋白在水中的溶解度显著增加,溶出的蛋白质的乳化容量先下降而后又趋上升。     

棉籽加工中棉粕蛋白质含量和棉籽油色泽的控制

主要叙述了以棉籽为原料,生产加工后得到两个主要产品——棉粕和棉籽油,分别分析了影响棉粕蛋白质含量和棉籽油色泽的因素,并提出了控制各因素的关键点。在实际生产中,通过控制这些关键因素,可得到高蛋白的棉粕和高品质的棉籽油。