凝胶渗透色谱净化-气相色谱法同时测定饲料中4种抗氧化剂

本文建立了凝胶渗透色谱净化(GPC)-气相色谱法(GC)同时测定饲料中2,6-二叔丁基对甲酚(BHT)、叔丁基羟基茴香醚(BHA)、叔丁基对苯二酚(TBHQ)和乙氧喹(EQ)4种抗氧化剂方法。4种抗氧化剂在10～400mg/L时与峰面积有良好的线性关系(r2>0.9999),检出限(3S/N)为0.37～0.46 mg/kg,添加回收率为82.7%～98.8%,相对标准偏差(n=5)为1.7%～4.3%。     

高效液相色谱法同时测定饲料中5种合成类抗氧化剂含量

本文旨在建立同时测定饲料中没食子酸丙酯(PG)、特丁基对苯二酚(TBHQ)、乙氧基喹啉(EQ)、丁基羟基茴香醚(BHA)和二丁基羟基甲苯(BHT)5 种合成类抗氧化剂含量的高效液相色谱法。 试样经超声波辅助乙腈直接提取,提取液经有机相针式滤器过滤净化后,采用十八烷基键合相(C₁₈)柱为色谱柱 (长 150 mm×内径 4.6 mm,粒径 5 μm),乙腈-2%乙酸溶液(65 + 35,V₁+V₂)为流动相 ,流速为 0.5 m L/min,检测波长为 280 nm,柱温为 20 ～ 30℃。 在此实验条件下,PG 在质量浓度 0.50 ～ 25.00 μg/mL,TBHQ、EQ、BHA 和 BHT 在质量浓度 1.00 ～ 50.00 μg/mL 内均与峰面积呈良好的线性关系(相关系数 r² > 0.999);PG、TBHQ、EQ、BHA 和 BHT 的检出限分别为 1.8、1.9、2.0、1.9、5.0 mg/kg,定量限分别为 8.8、8.6、8.9、8.7、10.0 mg/kg;PG、T...     

气相色谱-质谱法测定鸡蛋中三聚氰胺残留

采用气相色谱-质谱法(GC-MS)测定了鸡蛋中三聚氰胺残留。样品匀浆后,用三氯乙酸去蛋白提取,MCX柱净化,BSTFA和TMCS衍生化后,气相色谱-质谱检测。质谱定性离子为m/z342、327、171和99,定量离子为m/z327。方法定量限为0.5μg/g,添加浓度为0.5、2μg/g和10μg/g时的回收率在89.2%~96.2%之间,变异系数在2.9%~5.6%之间。     

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%。     

分散固相萃取-气相色谱-质谱方法快速检测奶牛饲料中的3种除草剂残留

建立了奶牛饲料样品中甲草胺、乙草胺、莠去津3种除草剂的气相色谱-质谱(GC-MS)检测方法,样品经分散固相萃取法处理后,取上清液用安捷伦HP-5气相色谱毛细管柱分离,气相色谱-质谱联用仪进行测定。3 种除草剂在 5~500 μg/kg 内线性关系良好。平均添加回收率为94.5%~115.4%,相对标准偏差(RSD) 为4.4%~9.2%,最低检测限为1.5 μg/kg。本方法前处理操作快速简单,可重复性好,满足国内外对饲料中甲草胺、乙草胺和莠去津的快速、准确的检测要求,适合大量样品的准确定量和定性分析。     

气相色谱法测定咸鱼中的敌百虫和敌敌畏

建立了咸鱼中敌百虫、敌敌畏农药残留的气相色谱分析方法。样品采用乙腈-水(1 1)溶液提取,加乙酸锌净化,用乙酸乙酯进行液液分配,最后采用DB-1701P或DB-5毛细管柱分离,使用气相色谱-火焰光度检测器分析。在4个添加水平的敌百虫、敌敌畏平均回收率(n=6)分别为91%~95%、90%~94.5%,相对标准偏差分别为3.82%~5.80%和3.57%~4.62%;方法的检出限为:敌百虫0.005 mg/kg,敌敌畏0.005 mg/kg。该方法可用于市场上咸鱼样品中敌百虫、敌敌畏的测定。     

气相色谱—质谱法测定饲料中四螨嗪的残留量

试验建立了气相色谱-质谱选择离子法(GC-MSD)测定饲料中四螨嗪残留量的检测方法。试样用水-丙酮(1 4)振荡提取,经二氯甲烷液-液分配,以凝胶色谱柱净化,再经氟罗里硅土(Florisil)固相柱净化,洗脱液浓缩并溶解定容后,供气相色谱-质谱仪检测,外标法定量。回收率范围为80.5%~99.0%;相对标准偏差为4.44%~9.64%;测定低限为0.010mg/kg。     

气相色谱法测定饲料中香芹酚和百里香酚的含量

文章建立了饲料中2种香料香芹酚和百里香酚的气相色谱检测方法。样品中香芹酚和百里香酚经乙酸乙酯超声提取90 min,经GCB和PSA净化后,用GC-FID测定。在1~500μg/ml的浓度范围内,香芹酚和百里香酚的峰面积响应与其浓度呈线性相关(R≥0.99),香芹酚和百里香酚定量限为10 mg/kg,在10种饲料中3个不同添加浓度的回收率为77.97%~104.04%,RSD为0.63%~9.92%,并通过气质联用仪进行确证。     

凝胶渗透色谱净化-气相色谱分离同时测定饲料中30种有机磷农药残留

文中建立了凝胶渗透色谱净化-气相色谱法同时测定饲料中敌敌畏、乐果等30种有机磷农药残留的方法。饲料样品用乙腈体系提取,采用凝胶色谱柱净化,毛细管色谱柱分离(DB-50+,30 m×0.25 mm×0.25μm),火焰光度检测器(FPD)检测,外标法定量。其方法检测限为5.6~54μg/kg,三水平添加回收率为71.3%~114.1%,RSD为0.3%~14.8%。方法简便、准确,并能满足饲料中多种有机磷农残测定的需要。     

气相色谱-串联质谱法检测鸭组织中哌嗪的残留

建立了气相色谱-串联质谱法检测鸭组织(肌肉、肝脏、肾脏以及皮肤和脂肪)中哌嗪残留的新方法。样品通过加速溶剂萃取(ASE)和固相萃取(SPE)提取、净化,乙酸酐法衍生化后用气相色谱-串联质谱(GC-MS/MS)检测和确证。采用EI模式,SCAN和SIM扫描定性,Auto SRM结合外标法定量。在定量限(LOQs),50,100,500,1 000和2 000μg/kg的加标水平上,鸭组织中哌嗪的平均回收率为84.24%~95.49%,相对标准偏差(RSDs)为2.03%~5.30%,日内相对标准偏差为1.72%~5.01%,日间相对标准偏差为2.11%~7.35%。哌嗪在鸭组织的检测限(LODs)为1.4~1.5μg/kg(S/N≥3),LOQs为4.8~5.2μg/kg(S/N≥10),其显著低于最大残留限量(MRL)。此方法灵敏度高,定性、定量准确,适用于鸭组织中哌嗪残留的确证检测。     

Stability of abdominal fat and meat of broilers: Relative effects of vitamin E,butylated hydroxytoluene and ethoxyquin 1

1. α‐Tocopheryl acetate (ATA) and ethoxyquin (EQ) markedly improved the stability of fat and meat of broilers fed on diets not supplemented with fat, while butylated hydroxytoluene (BHT) improved fat stability only.

2. The stability of carcass fat of broilers fed on diets supplemented with acidulated soyabean‐oil soapstock was improved by all three anti‐oxidants, but BHT and EQ were more effective than ATA. Meat stability was improved only by EQ.

3. The relationship between dietary EQ concentrations and the stability of carcass fat was logarithmic, whereas with that of thigh meat it was linear, irrespective of the degree of saturation of the carcass fat.     

HPLC-PDA法测定兽用中药液体制剂中非法添加的四种解热镇痛类药物

实验建立了兽用中药液体制剂中非法添加对乙酰氨基酚、安乃近、氨基比林、安替比林四种解热镇痛类药物的高效液相色谱-二极管阵列(HPLC-PDA)检测方法.方法采用CAPCELL PAK MGⅡS5 C18(4.6 mm×150 mm,5μm)色谱柱,柱温30℃,流动相为磷酸盐缓冲液和乙腈(84:16),流速1.0 mL/m...     

QuEChERS-dSPE-UPLC-MS/MS筛查中药材地龙中41种兽药残留

建立了基于超高效液相色谱串联三重四极杆质谱(UPLC-MS/MS)的动态多反应监测模式(d-MRM)快速筛查中药材地龙中7大类(喹诺酮类、磺胺类、糖皮质激素类、硝基咪唑类、抗病毒类、非甾体抗炎类、镇静安眠类)41种兽药残留的分析方法。样品采用QuEChERS提取,分散式固相萃取管(dSPE EMR-Lipid)进行净化,采用d-MRM采集模式进行定性和定量检测,外标法定量,41种兽药测定在各自线性范围呈良好的线性关系,相关系数(R 2)均大于0.9917,检出限为0.1000~3.105μg/kg,定量限为0.3184~7.532μg/kg,3个添加水平的回收率为62.8%~112.3%,精密度为1.1%~8.9%。该方法前处理简单、重现性好、灵敏度高,适用于中药材地龙中41种兽药残留的快速筛查。     

蜂王浆中小分子物质BHT的抗氧化活性研究

为深入探讨蜂王浆的抗衰老功能因子,分别采用邻苯三酚法和Fenton法测定了蜂王浆中存在的2,6-二叔丁基-4-甲基苯酚(BHT)对超氧阴离子和羟自由基的清除率,结果证实BHT对超氧阴离子和羟自由基有很强的清除力,当BHT的浓度达到600mg/L时,对超氧阴离子的清除率达75.86%,为最强;当BHT的浓度达到500mg/L时,对羟自由基的清除率达到84.47%,为最强。     

Testing Usability of Butylated Hydroxytoluene in Conservation of Goat Semen

The objective of this study was to investigate whether butylated hydroxytoluene (BHT) could be used as a suitable supporter or alternative of egg yolk during preservation of goat spermatozoa. Three in vitro experiments and a fertility test were conducted to evaluate the effect of BHT on viability of chilled‐stored semen as well as motility and kidding rate of frozen‐thawed spermatozoa. In the first two experiments, ejaculates (n = 30/experiment) were collected from 10 bucks, split, diluted with egg yolk‐based and egg yolk‐free extenders supplemented with or without 0.3, 0.6, 2, 5 and 8 mm BHT and stored at 5°C for 168 h. In the third experiment, 30 ejaculates were collected from the above‐mentioned bucks, split and diluted with egg yolk‐free extenders supplemented with or without 0.3, 0.6 and 0.9 mm BHT and egg yolk‐based extenders supplemented with or without 5 mm BHT. Diluted semen was cooled to 5°C over a period of 4 h, frozen and thawed in the form of 0.3‐ml pellets. In the fertility test, 75 ejaculates were collected from two proven fertile bucks, split, diluted with egg yolk‐free extenders containing 0.6 mm BHT and egg yolk‐based extenders supplemented with or without 5 mm BHT, frozen and thawed as described above. An insemination volume of 0.6 ml containing 120–140 × 10⁶ progressively motile spermatozoa was used for a single cervical insemination of cloprostenol‐synchronized does (n = 230). The results showed that addition of 5 mm BHT to egg yolk‐deficient (2.5%) extenders significantly improved viability of chilled‐stored semen together with motility (48.5%) and fertility (62.5%) of frozen‐thawed spermatozoa. Replacement of egg yolk in semen extenders by 0.6 mm BHT could sustain not only viability of chilled‐stored semen but also post‐thaw motility (47.5%) and fertility (53.75%) of frozen‐thawed spermatozoa. In conclusion, supplementation of semen diluents with BHT can ameliorate preservability of goat sperm.     

HPLC-PDA法同时测定黄芪多糖注射液中非法添加的四种解热镇痛类药物

采用迪马钻石C18(250 mm×4.6 mm,5μm)柱,以磷酸盐缓冲液(磷酸二氢钠6.0g,加水1000 mL使溶解,加三乙胺1mL,用氢氧化钠试液调pH值至7.0)-甲醇(70∶30,V/V)为流动相,流速1.0 mL/min,建立了同时测定黄芪多糖注射液中非法添加四种解热镇痛类药物的HPLC-PDA法.结果显示,在该色谱条件下四种解热镇痛类药物得到良好分离,在测定范围内线性关系良好,检测限1 ～4 μg/mL,定量限5～10 μg/mL,回收率均大于99.0％.本方法简便、灵敏、准确、快速、重现性好,可对黄芪多糖注射液中非法添加的四种解热镇痛类违禁药物进行定性和定量检测.     

HPLC法同时测定芩黄颗粒中黄芩苷和甘草酸的含量

建立了高效液相色谱法(HPLC)同时测定芩黄颗粒中黄芩苷和甘草酸的含量。采用Agilent Eclipse XDB-C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.05%磷酸溶液为流动相,梯度洗脱,检测波长为252 nm,流速为1.0 mL/min。结果显示,黄芩苷和甘草酸的进样浓度分别在61.84~618.4、8.256~82.56μg/mL(R 2=0.9999,0.9999)范围内与峰面积呈良好线性关系;精密度、重复性和稳定性试验的RSD均小于2.0%;平均加样回收率分别为100.0%、99.2%,回收率的RSD分别为1.0%、0.6%(n=6)。本方法操作简便、准确,可用于芩黄颗粒中黄芩苷和甘草酸含量的同时测定。     

Protective effects of antioxidants on bitterweed (Hymenoxys odorata DC) toxicity in sheep

Antidotal effects of the 2 antioxidants butylated hydroxyanisole (BHA) and ethoxyquin (EQ) were evaluated in bitterweed (Hymenoxys odorata DC) toxicosis in sheep. Bitteerweed contains a toxic sesquiterpene lactone, hymenoxon, the toxicity of which is reduced by cysteine. Both BHA and EQ are known to induce hepatic glutathione production in rodents. Treatment of sheep with EQ (2.5 g/sheep/day for 9 days before poisoning) gave significant protection from toxic doses of bitterweed, but the protective effect of BHA was insignificant. Of 6 sheep given EQ in the feed, 5 survived 7 doses of bitterweed (4 g/kg/day or higher for 7 days), whereas 5 of 7 controls and 4 of 7 sheep given feed with added BHA died. The added EQ in the feed decreased the serum alkaline phosphatase activity and total protein, albumin, and calcium concentrations. Seemingly, EQ is the first protective agent with field application potential for bitterweed toxicity.     

超高效液相色谱法测定鳗鱼中氟乐灵残留量

建立了一种超高效液相色谱法测定鳗鱼中氟乐灵残留量的方法.样品经正己烷均质提取,浓缩后经弗罗里硅土小柱净化,浓缩,甲醇定容,超高效液相色谱分离,TUV检测器检测,以保留时间定性,以峰面积定量.结果表明:在0.05～5μg/mL范围内浓度与峰面积线性关系良好,相关系数r=0.999 97;在0.01～0.5 mg/kg添加...     

Effect of butylated hydroxytoluene on dog sperm longevity in chilling storage and cryopreservation

This study evaluated the effect of butylated hydroxytoluene (BHT), a lipid-soluble antioxidant, on dog sperm in chilling storage and cryopreservation. In Experiment 1, 0.2, 0.4, 0.8 and 1.6 mM BHT were added to egg yolk Tris extender (EYT), and sperm were stored at 4°C for 96 hr. Sperm motility, viability, acrosomal integrity and morphological abnormality in the BHT treatment groups were not different from those of the control (0 mM BHT). In Experiment 2, the effect of BHT in EYT containing 0.75% Equex STM paste and 5% glycerol on survivability of cryopreserved sperm was examined after culture at 39°C for 3 hr. Sperm motility, viability and acrosomal integrity in the 0.2 to 0.8 mM BHT treatment groups were not different from those of the control. However, sperm motility, viability and acrosomal integrity decreased when 1.6 mM BHT was added to the extender (P<0.05). In conclusion, supplementation of the extender with 0.2 to 0.8 mM BHT did not affect characteristics of dog sperm in chilling storage and cryopreservation. Supplementation of 1.6 mM BHT did not affect characteristics of chilled sperm but impaired longevity of cryopreserved sperm in the dog.