毛细管胶束电动色谱法检测饲料中防腐剂

建立了同时分离测定山梨酸(SA)、苯甲酸(BA)、对羟基苯甲酸甲酯(MP)、对羟基苯甲酸乙酯(EP)、对羟基苯甲酸丙酯(PP)、对羟基苯甲酸丁酯(BP)6种防腐剂的胶束电动毛细管色谱方法。以十二烷基硫酸钠(SDS)-磷酸盐-硼砂缓冲体系为缓冲液,pH为7.73,电压为20 kV,于245 nm波长下对样品进行检测。结果表明,6种防腐剂均在14 min内实现很好分离,SA、BA的线性范围分别为0.5～150μg/mL和15～200μg/mL,MP、EP的线性范围均为2～200μg/mL,PP的线性范围为5～200μg/mL,BP的线性范围为1～200μg/mL,线性相关系数为0.9987～0.9995,平均回收率为89.7%～96.7%,RSD≤5.91%,检测限为0.25～10μg/mL。     

超高效液相色谱法测定饲料中斑蝥黄和β-阿朴-8’-胡萝卜素酸乙酯含量方法的研究

为有效快速测定饲料中斑蝥黄和β-阿朴-8’-胡萝卜素酸乙酯含量,饲料经甲醇、正己烷和乙酸乙酯混合液萃取后,在氮气保护下浓缩,用甲基叔丁基醚-乙腈溶液复溶,注入超高效液相色谱仪中进行测定。结果表明:斑蝥黄浓度为1.25~10.0μg/mL,β-阿朴-8’-胡萝卜素酸乙酯为2.50~20.0μg/mL线性关系良好;斑蝥黄和β-阿朴-8’-胡萝卜素酸乙酯的检测限为0.06 mg/kg,定量限为0.20 mg/kg。斑蝥黄5个添加水平的平均回收率为72.8%~82.8%,相对标准偏差(RSD)为0.41%~1.06%;β-阿朴-8’-胡萝卜素酸乙酯5个添加水平的平均回收率为72.0%~82.8%,RSD为0.46%~1.41%。说明该方法简便、快速、灵敏度高、准确度好,适用于测定饲料中斑蝥黄和β-阿朴-8’-胡萝卜素酸乙酯含量。     

固相萃取-反相高效液相色谱法测定蛋黄中的斑蝥黄

本试验旨在建立一种定量测定蛋黄中斑蝥黄的固相萃取-反相高效液相色谱法。蛋黄用乙腈在超声波辅助下提取,提取液经过Oasis~? PRiME HLB固相萃取柱净化,再由C_(18)色谱柱分离,流动相为乙腈-水(95∶5,体积比),流速为1.2 mL/min,等度洗脱,在紫外-可见吸收波长474 nm处检测,外标法定量。结果显示:蛋黄中斑蝥黄的检出限为0.05μg/g,定量限为0.1μg/g。斑蝥黄在0.1～10.0μg/mL的浓度范围内线性关系良好,相关系数(R~2)为0.999 9。在3个加标浓度(0.1、1.0和4.0μg/g)下,斑蝥黄的回收率为85.9%～98.6%,相对标准偏差(RSD)为1.7%～8.0%。应用上述方法测得市售新鲜鸡蛋蛋黄中斑蝥黄含量高达8.3μg/g。本试验建立的固相萃取-反相高效液相色谱法能够满足蛋黄中斑蝥黄及其异构体快速定量的需要。     

高效毛细管电泳法同时检测饲料中六种抗氧化剂

实验以25 mmol/L硼砂-硼酸(Na2B4O7-H3BO3)和10 mmol/L十二烷基硫酸钠(SDS)的混合液(pH=7.00)作为缓冲液,采用高效毛细管胶束电动色谱法测定样品中丁基羟基茴香醚(BHA)、二叔丁基甲基苯酚(BHT)、特丁基对苯二酚(TBHQ)、没食子酸异丙酯(PG)、没食子酸辛酯(OG)、乙氧基喹啉(EQ)六种抗氧化剂。该方法在15 min内实现了六种抗氧化剂的分离;TBHQ和BHA的线性范围为50～500μg/mL,PG、EQ、OG和BHT的线性范围分别为10～200、20～200、25～400μg/mL和25～500μg/mL,线性相关系数≥0.996。TBHQ、PG、BHA、OG、EQ、BHT的检测限分别为30、5、25、15、10、10μg/mL;样品平均回收率为81.8%～102.0%,相对标准偏差≤6.5%。     

分子印迹固相萃取-高效液相色谱法检测饲料中联苯三唑醇

实验建立了分子印迹固相萃取-高效液相色谱法检测饲料中联苯三唑醇。采用本体聚合法自制联苯三唑醇分子印迹聚合物(MIP),并以此聚合物为固相萃取剂,对饲料样品中联苯三唑醇进行了分离富集。利用高效液相色谱法测定其在饲料中的残留情况。结果表明:该方法线性范围为1～200μg/mL,检测限为0.5μg/mL,平均回收率为76.4%～89.0%。     

农村散养土鸡机体组织和鸡蛋中类胡萝卜素成分研究

为研究农村散养土鸡机体组织和鸡蛋中类胡萝卜素成分，试验选取100只农村散养土鸡，同时收集100枚土鸡蛋，通过比色法及高效液相色谱法测定土鸡机体组织和土鸡蛋蛋黄的色度及类胡萝卜素含量。试验结果表明：（1）土鸡蛋蛋黄色度8 ～ 14度|蛋黄中类胡萝卜素含量丰富，总叶黄素28.83 ～ 106.94 mg/kg，主要以黄体素和玉米黄质为主，同时也含有斑蝥黄、β-胡萝卜素、虾青素和辣椒红素等|（2）土鸡脚蹼色度1 ～ 6度，总叶黄素6.78 ～ 43.88 mg/kg，主要是黄体素、玉米黄质和斑蝥黄等|（3）土鸡脚胫色度2 ～ 8度，总叶黄素14.59 ～ 58.22 mg/kg，主要是黄体素、玉米黄质、斑蝥黄和辣椒红素等|（4）土鸡皮肤色度1 ～ 6度，总叶黄素4.68 ～ 5.29 mg/kg，主要是黄体素、玉米黄质、斑蝥黄和辣椒红素等|（5）土鸡脂肪色度4 ～ 12度，总叶黄素4.55 ～ 7.38 mg/kg，主要是黄体素、玉米黄质、斑蝥黄、β-阿朴酯和辣椒红素等。结果说明，色泽越深的组织样品，其类胡萝卜素含量越丰富|同时也得出公鸡机体各部分色泽均比母鸡深，说明公鸡着色能力比母鸡强。 [关键词] 散养土鸡|土鸡蛋|类胡萝卜素|成分研究     

复合预混合饲料中β-胡萝卜素测定方法研究

本文采用高效液相色谱法建立复合预混合饲料中β-胡萝卜素含量的测定方法。样品经皂化萃取浓缩后,用Aglient C18色谱柱,甲醇-异丙醇-二氯甲烷为流动相,在450 nm检测,外标法定量。结果表明:β-胡萝卜素在0～10μg/mL有较好的线性关系,r~2均大于0.999。方法中β-胡萝卜素线性关系良好,检出限为1 mg/kg,回收率为95%～102%,相对标准偏差小于6%。该方法具有稳定性好、灵敏度高等优点,适用于复合预混合饲料中β-胡萝卜素含量的检测。     

高效液相色谱法测定加米霉素原药含量的研究

为建立测定加米霉素含量的高效液相色谱法,试验应用资生堂CAPCELL PAK C18 MGⅡ(250×4.6mm,5μm)色谱柱,色谱乙腈溶解样品,色谱条件以磷酸盐缓冲液(取0.01mol/L磷酸氢二钾溶液,用20%磷酸溶液调节pH值至8.0)-乙腈(20:80)为流动相,检测波长为210nm;流速为1.0mL/min;柱温为40℃。结果:加米霉素的线性范围为1.714μg/mL～450μg/mL,四批样品中加米霉素的含量分别是99.14%、99.20%、99.33%、99.41%。结论:该检测方法准确、简单、灵敏度高、分离效果好,适用于加米霉素原料的检测。     

高效液相色谱法测定羊血液中三聚氰胺

试验建立了应用高效液相色谱测定羊血液中三聚氰胺含量的方法。样品经三氯乙酸-乙酸锌提取,MCX固相萃取柱净化后,应用DikmaC18色谱柱进行分离,缓冲液为辛烷磺酸钠和柠檬酸混合溶液,以缓冲液+乙腈为流动相,流速为1mL/min,柱温25℃,紫外检测波长为240nm。定量分析采用外标法,线性范围为0.5～100μg/mL,线性方程为y=2939.6x+160.59,相关系数(R2)=0.9999,样品添加回收率范围为81.4%～93.1%,变异系数为1.87%～3.29%,检测限为0.5mg/kg。     

海南热带植物叶黄素和β-胡萝卜素含量分析

应用高效液相色谱法分析海南113种热带植物的叶黄素和β-胡萝卜素含量。结果表明:叶黄素含量>1000mg/kg者44种,500mg/kg<叶黄素含量<1000mg/kg者42种,200mg/kg<叶黄素含量<500mg/kg者21种、在200mg/kg以下者6种;β-胡萝卜素含量>50g/kg者33种、20g/kg<β-胡萝卜素含量<50g/kg者65种、小于20g/kg者15种;研究结果对热带植物类胡萝卜素资源综合开发与利用者有一定参考价值。     

Chromatographic analysis of lypophilic compounds in eggs from organically fed hens

Egg yolks represent a common foodstuff in the human diet and are an important source of nutrients including lipids and carotenoids. The aim of this study was to compare the carotenoid, fatty acid and vitamin E contents of the yolk of eggs from nine hen breeds (Barred Plymouth Rock, Speckled Italian, Black Italian, Red Italian, Rhode Island, Silver Laced Wyandotte, Gold Araucana, Partridge Brahma and Yellow Cochin) raised in barns in an enclosed house. Gas chromatography-mass spectrometry (GC-MS) was used for the fatty acid analyses, and reversed phase-high performance liquid chromatography-photodiode array detection (RP-HPLC-PDA) for carotenoids and vitamin E quantification. The major carotenoids identified were lutein and zeaxanthin, which together represented more than 93% of the total carotenoids, followed by β-cryptoxanthin and β-carotene.The results indicated that the total carotenoid content of the eggs ranged from 16.84–87.31 μg/g egg yolk (average value 49 μg/g egg yolk). The most representative fatty acids found were palmitic acid, stearic acid, oleic acid and linoleic acid. Significant differences in the proportions of α-linolenic acid were observed among the samples. The α-tocopherol content was directly correlated with the total carotenoid content. The results show that the chemical composition of egg yolk varies greatly among hen breeds.     

Reduction of deoxynivalenol contaminating corn silage by short-term ultraviolet irradiation: a pilot study

We evaluated the effects of short-term (up to 60 min) irradiation of corn silage with ultraviolet (UV) light (intensity: 1.5 mW/cm(2) at 254 nm UV-C wavelength), along with constant stirring of the silage, on the concentration of deoxynivalenol (DON), a major feed-contaminating mycotoxin, and those of α-tocopherol (vitamin E) and β-carotene (pro-vitamin A). The initial DON concentration in artificially contaminated silage was set at approximately 60 μg/g dry silage weight. After irradiation, the level of DON was decreased significantly (P<0.05) by approximately 13 μg/g (22%) on average at 30 min, and by 12 μg/g (21%) at 60 min. However, the concentrations of the vitamins remained relatively unaffected. Although further improvement is needed, short-term UV irradiation seems a promising on-farm method for reducing the level of DON in feedstuffs.     

高效液相色谱法测定恩诺沙星、盐酸小檗碱粉中两种有效成分含量

建立了恩诺沙星、盐酸小檗碱粉中两种有效成分含量的高效液相色谱测定法。采用C18色谱柱（4.6 mm×250 mm,5μm）,检测波长265 nm,流动相为乙腈-0.005 moL/L庚烷磺酸钠溶液（用磷酸调节pH值至3.0）（40∶60）,流速1.0 mL/min。结果显示,恩诺沙星在10.0～200.0μg/mL范围内含量与峰面积呈良好的线性关系,相关系数为0.9999（n=6）,平均回收率101.3%,RSD为2.0%;盐酸小檗碱在5.0～100.0μg/mL范围内含量与峰面积呈良好的线性关系,相关系数为1.0000（n=6）,平均回收率97.0%,RSD为2.6%。本方法简便、准确、快速、重现性好,可用于该制剂的含量测定。     

The effect of tannic acid and polyethylene glycol on the absorption capacity of chicken intestine for d-xylose and β-carotene

In an experiment, the possible influence of tannic acid (TA) and polyethylene glycol (PEG) on the absorption capacity of intestine for d-xylose and β-carotene in broiler chicken was investigated. Four groups of nine 28-day-old broiler cockerels received d-xylose (500 mg) and β-carotene (52 μg) solutions (Group 1 to 4) with TA (1 g, Group 2 to 4) and PEG (500 mg Group 3 and 1 g Group 4), orally. One blood sample prior to, and four others after the administration of test materials, were collected from wing vein on 40 min basis, for 160 min and the concentration of plasma d-xylose was determined. The concentration of β-carotene was also measured in plasma of blood samples taken prior to and 160 min post-administration of the test materials. Plasma d-xylose concentration of all groups showed quadratic correlations with time (p < 0.001, r(2) = 0.84, 0.60, 0.70 and 0.74 for Group 1 to 4, respectively). Administration of TA reduced the plasma concentration of d-xylose in Group 2. However, feeding PEG after TA raised the concentration of d-xylose in Group 4 to the level that there was no difference in that variable between this group and Group 1. Although the plasma concentration of β-carotene was increased in 160 min post-ingestion of the test material, no difference was found in that variable among the experimental groups. In conclusion, TA and its interaction with PEG have impacts on the absorption capacity of intestine for d-xylose and highly likely other simple sugars, but TA or PEG have no influence on the absorption of β-carotene and most probably other fat soluble vitamins.     

HPLC测定盐酸多西环素可溶性粉含量

采用高效液相色谱法(HPLC)测定盐酸多西环素可溶性粉中多西环素的含量,并对检验方法[1]进行复核验证.色谱柱 Waters Nova.pakR○C18( 3.9 mm×150 mm, 4 μm);以0.05 mol/L草酸铵溶液-二甲基甲酰胺-0.2 mol/L磷酸氢二铵溶液(65∶30∶5)(用氨试液调节pH值为8.0)为流动相;柱温35 ℃;检测波长280 nm;流速1.0 mL/min;进样量20 μL.多西环素进样浓度在4.0～144.0 μg/mL的范围内与峰面积呈良好的线性关系(r=1.000);样品的平均加样回收率(n=9)为98.5%,RSD为2.0%;完成了185批次样品的检验,检验结果准确可靠.该方法准确度高,重复性好,结果可靠,能够有效地检测盐酸多西环素可溶性粉的含量.     

HPLC法测定复方替米考星颗粒中有效成份含量

采用HPLC法同时测定了复方替米考星颗粒中替米考星、磺胺二甲氧嘧啶及甲氧苄啶的含量。色谱柱为Eclipse XCB-C18(250 mm×4.6 mm,粒径5μm),流动相为磷酸二丁胺缓冲液-乙腈-四氢呋喃-水(25∶115∶55∶805),检测波长280 nm,流速1.0 mL/min。出峰顺序为甲氧苄啶、磺胺二甲氧嘧啶、替米考星反式结构、替米考星顺式结构,理论塔板数分别为7963、15714、3282、8701。两峰之间的分离度分别为24.29、3.92、2.91;拖尾因子分别为0.92、0.90、0.97、0.94。替米考星、磺胺二甲氧嘧啶、甲氧苄啶的浓度线性范围分别是6.25～125μg/mL(R2=0.996),3.125～62.5μg/mL(R2=0.996),0.625～12.5μg/mL(R2=0.999);平均回收率分别为99.17%、99.06%和99.39%;RSD分别为0.8%、0.9%和0.9%。该法快速、灵敏、准确,适用于同时测定复方替米考星颗粒中三种成份的含量。     

盐酸特比萘芬对家蚕真菌病的防治效果试验初报

以家蚕真菌病病原为受试菌,对抗真菌药物氟康唑(FCZ)和盐酸特比萘芬(TBF·HCl)进行了体外筛选,研究了盐酸特比萘芬对家蚕真菌病的防治效果及其稳定性。试验结果表明,盐酸特比萘芬的体外抑菌、杀菌效果优于氟康唑,盐酸特比萘芬对家蚕病原真菌的最小抑菌浓度范围为0.0625～0.2726μg/mL,最小杀菌浓度范围为0.125～4μg/mL。生物试验表明,盐酸特比萘芬对家蚕真菌病防治效果良好,200μg/mL时防治效果达100%,且对家蚕生长发育、茧质无不良影响。稳定性试验表明盐酸特比萘芬长期稳定性良好。     

Effects of oral supplementation with β-carotene on concentrations of β-carotene, vitamin A and α-tocopherol in plasma, colostrum and milk of mares and plasma of their foals and on fertility in mares

In this study, effects of oral β-carotene supplementation to mares (β-carotene group: 1000 mg/day, n = 15; control group: n = 15) from 2 weeks before foaling until 6 weeks thereafter on concentrations of β-carotene, vitamin A and α-tocopherol in plasma, colostrum and milk and plasma of their foals were determined. In addition, effects on fertility were studied. Beta-carotene concentrations increased in plasma and colostrum of β-carotene-supplemented mares compared to control mares (p < 0.05). In mares of both groups, β-carotene concentrations were higher in colostrum than in milk (p < 0.05). In foals, β-carotene concentrations increased with colostrum uptake and were higher in foals born to supplemented mares (p < 0.05; control group: 0.0003 ± 0.0002 μg/ml on day 0, 0.008 ± 0.0023 μg/ml on day 1; β-carotene group: 0.0005 ± 0.0003 μg/ml on day 0, 0.048 ± 0.018 μg/ml on day 1). Concentrations of vitamin A and α-tocopherol were higher in colostrum than in milk (p < 0.05) but did not differ between groups. Concentration of α-tocopherol in plasma of mares decreased over time and in foals, increased markedly within 4 days after birth. All but one mare (control group) showed oestrus within 2 weeks post-partum. Occurrence of oestrus did not differ between groups. More mares of the control group (7/7 vs. 5/12 in the β-carotene group) became pregnant after being bred in first post-partum oestrus (p < 0.05). In conclusion, β-carotene supplementation to mares increased β-carotene concentrations in plasma, colostrum and milk of mares and plasma of their foals but had no positive effects on fertility.