液相色谱-串联质谱法测定鸡蛋中氟虫腈及其代谢物的残留量

建立一种采用液相色谱-三重四级杆质谱测定鸡蛋中氟虫腈及其代谢物(氟甲腈、氟虫腈砜和氟虫腈硫醚)的快速筛查方法。鸡蛋样品经乙腈和正己烷提取,C18固相萃取柱净化,Shim-pack XR-ODSⅢ色谱柱(2.0 mm i.D×150 mm,2.1μm)分离,以乙腈-5 mmol/L乙酸铵(0.02%甲酸)水溶液为流动相,梯度洗脱,外标法定量。采用液相色谱-三重四级杆串联质谱动态多反应监测模式,以负离子采集进行定性筛查和定量分析。结果表明,氟虫腈及其代谢物在0～50μg/L质量浓度范围内线性关系良好,相关系数R2均大于0.999。以10倍信噪比确定各药物的定量限(LOQ),氟虫腈及其代谢物的定量限为0.3～0.6μg/kg。在0.5、5.0和10.0μg/kg添加水平下,氟虫腈及其代谢物的平均回收率为92.3%～105.1%,相对标准偏差(RSD)为1.2%～8.6%。该方法简便、快速、灵敏,适用于鸡蛋中氟虫腈及其代谢物的快速筛查和定量检测。     

气相色谱法和高效液相色谱-串联质谱法测定 鸡蛋中氟虫腈及代谢物残留

目的建立适用于鸡蛋中氟虫腈及其代谢物(氟虫腈砜、氟虫腈硫醚和氟甲腈)残留的电子捕获检测器-气相色谱法和高效液相色谱-串联质谱检测方法。方法通过Qu ECh ERS提取盐包(CEN EN-15662)用乙腈提取目标化合物,借助固相萃取(PRiMEHLB)作为净化手段,采用气相和液相质谱进行监测。结果气相色谱法和高效液相色谱-串联质谱法中4种分析物的定性限(limit of detection,LOD)分别为0.1μg/kg和0.02μg/kg;定量限(limit of quantification,LOQ)分别为0.5μg/kg和0.1μg/kg,在0.1~10.0μg/L和0.1~5.0μg/L范围内线性关系良好,相关系数r~2均大于0.999。在2.5,5和10μg/kg 3种加标浓度下,平均回收率分别为80.8%~103%和87.4%~101%,相对标准偏差(relative standard deviation,RSD,n=6)分别为0.84%~5.62%和0.87%~4.40%。结论该方法步骤简便、可靠、稳定,适合于蛋类中氟虫腈及其代谢物残留的痕量分析。     

超高效液相色谱-串联质谱法测定鸡蛋中多种药物残留

建立鸡蛋中氯霉素类药物与氟虫腈及其代谢物的多残留同时检测的超高效液相色谱-串联质谱方法。以酸化乙腈为提取液,采用PRIME HLB净化的方式,超高效液相色谱-串联质谱法(HPLC-MS/MS)进行分析,多反应监测运行模式(MRM),电喷雾负离子模式,以甲醇水为流动相。该方法在0.005～10 μg/L线性关系良好,决定系数在0.99907～0.99995,定量限范围为0.01～0.08 μg/kg,平均回收率为93.5%～116.0%,相对标准偏差RSD值1.6%～8.8%。该方法过程简单,适用于鸡蛋中氯霉素类与氟虫腈及其代谢物的同时检测。     

气相色谱三重四极杆串联质谱法测定鸡蛋和鸡肉中氟虫腈及其代谢物残留量的研究

目的建立一种鸡蛋和鸡肉组织中氟虫腈及其代谢物残留的气相色谱三重四极杆串联质谱法(GC-MS/MS)检测方法。方法样品经乙腈提取液,Bond Elut EMR-Lipids法净化,去除鸡肉和鸡蛋组织中的脂类和蛋白质。质谱采用多反应监测模式(multiple reaction monitoring,MRM)对氟虫腈及其代谢物的定量离子和定性离子进行监测。结果本方法中氟虫腈及其代谢物在20.0~1000μg/L的浓度范围内,线性良好,相关系数r~2大于0.994,在10、20、50μg/L水平上的平均回收率在91%~114.32%之间,相对标准偏差(relative standard deviation,RSD)为0.4%~7.8%(n=6),氟虫腈及其代谢物的检出限(S/N=3)为2.0~3.5μg/kg,定量限(S/N=10)为6.0~10.5μg/kg。结论该方法具有前处理简便快捷、净化效果佳、灵敏度高、成本低等特点,适用于鸡蛋和鸡肉中氟虫腈的快速确认及定量检测。     

固相萃取-高效液相色谱检测鸡蛋中氟虫腈及其代谢物

目的建立固相萃取-高效液相色谱法测定鸡蛋中氟虫腈农药及其主要的代谢物氟虫腈砜、氟虫腈亚砜、氟甲腈的分析方法。方法选用含1%甲酸的乙腈溶液(V:V)为提取溶剂,用石墨化碳黑/氨基固相萃取小柱萃取净化,用乙腈作洗脱剂,并在以甲醇-水(67:33,V:V)为流动相的条件下进行高效液相色谱检测。结果该方法的线性范围为0.3～10.0μg/g,4种目标物的检测限均在0.05～0.10μg/g之间。通过对实际鸡蛋样品加标检测,得到加标回收率在80.9%～115.8%之间,相对标准偏差均小于6.2%。结论该方法精密度较高、稳定性良好、操作简便,可用于鸡蛋样品中氟虫腈及其3种代谢物的测定。     

鸡蛋中氟虫腈及其代谢物残留分析方法

采用超高效液相色谱-串联质谱技术,以鸡蛋为研究对象,建立一种高效测定鸡蛋中氟虫腈及其代谢物残留测定方法。样品用乙腈提取,并通过固相萃取技术对样品进行净化处理,供超高效液相色谱-串联质谱仪进行检测。实验结果表明,该方法能够有效地分离和测定氟虫腈及其代谢物残留。在3 个不同的添加水平（0.005、0.010、0.020 mg/kg）下,4 种农药的回收率范围为81.3%～92.5%,相对标准偏差均低于5.5%。;在0.001～0.050 μg/mL 浓度范围内,线性关系良好,相关系数均大于0.990 4;氟虫腈、氟甲腈、氟虫腈砜与氟虫腈亚砜的检出限分别为0.001、0.002、0.002、0.002 mg/kg。该方法准确、灵敏、快速,可满足对鸡蛋中氟虫腈、氟甲腈、氟虫腈砜与氟虫腈亚砜4 种药物残留的检测需要。     

固相萃取-UPLC-MS/MS法测定牛奶中氟虫腈及其代谢物残留量

建立一种固相萃取-超高效液相色谱-串联质谱法同时测定牛奶中氟虫腈及其代谢物(氟甲腈、氟虫腈砜、氟虫腈硫醚)的分析方法。牛奶样品经提取和盐析,Oasis PRiME HLB固相萃取柱通过式净化后,以乙腈-水为流动相,HSS T3色谱柱(2.1mm×100 mm,1.8 μm)进行色谱分离,在电喷雾负离子模式下,多反应监测(MRM)方式进行测定,外标法定量。结果表明,氟虫腈及其代谢物在0.05~5.0 μg/L浓度范围内均呈良好的线性关系,相关系数r≥0.9976,方法检出限为0.01 μg/kg,定量限为0.05 μg/kg。在浓度分别为0.5、1、10 μg/kg加标水平下,4种化合物的回收率范围为80.6%~101%,相对标准偏差范围为1.0%~6.1%。该方法简单快捷、准确可靠,适用于牛奶中氟虫腈及其代谢物的同时测定。     

QuEChERS-超高效液相色谱-串联质谱法测定鸡蛋、鸡肉中氟虫腈及其代谢物残留

建立一种基于QuEChERS法提取,超高效液相色谱分离,串联四极杆质谱法检测鸡蛋、鸡肉中氟虫腈及其代谢物残留量的方法。样品经加水分散后,用乙腈提取,柠檬酸缓冲盐脱水,稀释后上机测定。待测物经BEH?C18色谱柱分离,以甲醇-5?mmol/L乙酸铵溶液（含0.1%甲酸）进行梯度洗脱,质谱法采用电喷雾电离,负离子多反应监测模式检测。基质加标曲线定量。氟虫腈及3?种代谢物的定量限为1?μg/kg,在1～100?μg/kg范围内线性关系良好。在鸡蛋、鸡肉基质中3?个不同添加水平下,平均回收率为87.6%～117.7%,变异系数为3.6%～9.9%。该方法快速、灵敏、准确,适合作为禽蛋等动物源性食品中,氟虫腈及其代谢物残留总量的测定。     

QuEChERS-超高效液相色谱-串联质谱法检测禽源性食品中氟虫腈及其代谢物

建立QuEChERS-超高效液相色谱-串联质谱检测禽源性食品中氟虫腈及其代谢物的方法。采用Plackett-Burman试验和Box-Behnken试验筛选和优化QuEChERS前处理方法中的显著影响因素。最终优化条件：样品用乙腈超声提取,后用NaCl、无水MgSO4盐析分层,提取液再用碳十八键合锆胶（Z-Sep+）、多壁碳纳米管进行净化,净化液用超高效液相色谱-串联质谱分析测定,采用基质加标曲线进行定量测定。结果表明,在鸡蛋、鸡肉、鸡肝基质中氟虫腈、氟甲腈、氟虫腈砜、氟虫腈亚的平均加标回收率在78.9%～113.5%之间,相对标准偏差在2.10%～7.60%之间,检出限在0.1～0.2 μg/kg之间,定量限为0.5 μg/kg。此方法可有效降低禽源性食品中基质效应,具有高灵敏度、精密度、准确度,可用于禽类食品中氟虫腈及其代谢物残留的快速定量测定。     

PRiME HLB固相萃取结合气相色谱-串联质谱法快速测定酸笋、酸豆角中氟虫腈及其代谢物残留量

目的 建立气相色谱-串联质谱法(gas chromatography- tandem mass spectrometry, GC-MS/MS)测定酸笋、酸豆角中氟虫腈及其代谢物（氟甲腈、氟虫腈硫醚、氟虫腈砜）残留量的分析方法。方法 称取5 g样品（酸笋、酸豆角）,加入10 mL乙酸乙酯及6 g氯化钠振荡提取1 min,离心后取3 mL上清液经PRiME HLB（hydrophilic-lipophilic balanced copolymer）通过式固相萃取柱净化,残留量采用气相色谱-串联质谱法进行检测。结果 本实验建立的氟虫腈及其代谢物残留测定方法,在0.5~10.0 ng/mL线性范围内,相关系数r2均大于0.9994,4种农药分析物在各自浓度范围内均呈现良好线性关系,方法定量限均为1.0 μg/kg。在阴性酸笋、酸豆角中加入低、中、高3个添加水平,平均加标回收率及相对标准偏差分别为91.7%~100.2%、0.7%~10.2%。结论 该方法操作便捷、高效、环境友好,适合于酸笋、酸豆角中氟虫腈及其代谢物残留量的筛查。     

Ovarian structures and circulating steroids in heifers and lactating cows in summer and lactating and dry cows in winter

Two experiments compared follicular and luteal development and circulating steroid concentrations from induced luteolysis to ovulation in lactating Holstein cows (n = 27; 40.0 +/- 1.5 kg milk/day) vs. nulliparous heifers (n = 28; 11 to 17 mo-old) during summer (Experiment 1), and in lactating (n = 27; 45.9 +/- 1.4 kg milk/d) vs. dry cows (n = 26) during winter (experiment 2). All females received PGF2,, 6 d after ovulation and were monitored until next ovulation by daily ultrasound and assay of serum progesterone (P4) and estradiol (E2). Every female was used two or three times. In Experiment 1, lactating cows had high incidence of multiple ovulation (63.5%) compared with heifers (1.3%). Among single ovulators, there was no difference in maximal size of ovulatory follicles between lactating cows and heifers (15.8 vs. 16.5 mm, respectively). However, lactating cows had lower peak serum E2 (8.6 vs. 12.1 pg/ml), took longer to ovulate after luteolysis (4.6 vs. 3.8 d), developed more luteal tissue volume (7,293.6 vs. 5,515.2 mm3), and had lower serum P4 on d 6 after ovulation (2.0 vs. 3.0 ng/ml) than heifers (data included multiple ovulators). In experiment 2, multiple ovulations were similar between lactating and dry cows (17.9 vs. 17.2%, respectively). Peak serum E2 was also similar between lactating and dry cows (7.6 vs. 8.5 pg/ml) although lactating cows had larger ovulatory follicles (18.6 vs. 16.2 +/- 0.4 mm). Lactating cows took longer to ovulate (4.8 vs. 4.2 d), developed more luteal tissue (7,599 vs. 5,139 +/- 468 mm3), but had similar serum P4 (2.2 vs. 1.9 ng/ ml) compared with dry cows. Therefore, lactating cows had similar or lower circulating steroid concentrations than dry cows or heifers, respectively, despite having larger ovarian structures.     

Fertilization and early embryonic development in heifers and lactating cows in summer and lactating and dry cows in winter

Two experiments in two seasons evaluated fertilization rate and embryonic development in dairy cattle. Experiment 1 (summer) compared lactating Holstein cows (n = 27; 97.3 +/- 4.1 d postpartum [dppl; 40.0 +/- 1.5 kg milk/d) to nulliparous heifers (n = 28; 11 to 17 mo old). Experiment 2 (winter) compared lactating cows (n = 27; 46.4 +/- 1.6 dpp; 45.9 +/- 1.4 kg milk/d) to dry cows (n = 26). Inseminations based on estrus included combined semen from four high-fertility bulls. Embryos and oocytes recovered 5 d after ovulation were evaluated for fertilization, embryo quality (1 = excellent to 5 = degenerate), nuclei/embryo, and accessory sperm. In experiment 1, 21 embryos and 17 unfertilized oocytes (UFO) were recovered from lactating cows versus 32 embryos and no UFO from heifers (55% vs. 100% fertilization). Embryos from lactating cows had inferior quality scores (3.8 +/- 0.4 vs. 2.2 +/- 0.3), fewer nuclei/embryo (19.3 +/- 3.7 vs. 36.8 +/- 3.0) but more accessory sperm (37.3 +/- 5.8 vs. 22.4 +/- 5.5/embryo) than embryos from heifers. Sperm were attached to 80% of UFO (17.8 +/- 12.1 sperm/UFO). In experiment 2, lactating cows yielded 36 embryos and 5 UFO versus 34 embryos and 4 UFO from dry cows (87.8 vs. 89.5% fertilization). Embryo quality from lactating cows was inferior to dry cows (3.1 +/- 0.3 vs. 2.2 +/- 0.3), but embryos had similar numbers of nuclei (27.2 +/- 2.7 vs. 30.6 +/- 2.1) and accessory sperm (42.0 +/- 9.4 vs. 36.5 +/- 6.3). From 53% of the flushings from lactating cows and 28% from dry cows, only nonviable embryos were collected. Thus, embryos of lactating dairy cows were detectably inferior to embryos from nonlactating females as early as 5 d after ovulation, with a surprisingly high percentage of nonviable embryos. In addition, fertilization rate was reduced only in summer, apparently due to an effect of heat stress on the oocyte.     

Zinc and iron contents and their bioaccessibility in cereals and pulses consumed in India

Several cereals and pulses commonly consumed in India were screened for zinc and iron contents and their bioaccessibility in the same was determined by equilibrium dialysis employing an in vitro simulated digestion procedure. Zinc content of cereals ranged from 1.08 mg/100 g in rice to 2.24 mg/100 g in sorghum. Zinc content of pulses was between 2.03 mg/100 g (whole chickpea) and 2.68 mg/ 100 g (decorticated chickpea). Iron content of cereals ranged from 1.32 mg% in rice to 6.51 mg% in sorghum, while that of pulses ranged from 3.85 mg% in decorticated green gram to 6.46 mg% in black gram. Dialyzability of zinc from pulses (27–56%) was generally higher than that from cereals (5.5–21.4%). Dialyzabilities of iron were almost similar from both cereals and pulses examined and were 4.13–8.05% in cereals and 1.77–10.2 % in pulses. A significant negative correlation between inherent phytate content and zinc dialyzability value was inferred in the case of pulses. Phytic acid content of the cereals had a significant negative influence on iron dialyzability. Inherent calcium had a negative influence on zinc dialyzability in cereals. Tannin did not have any significant influence on zinc or iron dialyzabilities from cereals and pulses. While both insoluble and soluble fractions of the dietary fibre generally interfered with zinc dialyzability, the insoluble fraction alone had this effect on iron dialyzability. The lower collective negative influence of the inherent factors on zinc dialyzability from pulses is consistent with their higher concentrations in these grains, relative to cereals. The negative correlation of inherent phytic acid with zinc and iron dialyzabilities was supported by enhanced dialyzabilities of these minerals upon partial removal of phytate from the grains by treatment with fungal phytase.     

Fenvalerate residue level and dissipation in tea and in its infusion

Fenvalerate is a non-systemic insecticide/acaricide used in controlling a wide range of pests, including those resistant to organochlorine, organophosphorus and carbamate insecticides. The study investigated the dissipation behaviour (residue level) of fenvalerate in tea and its transfer during infusion. Fenvalerate was applied on tea crop at two dosages, 100 and 200?g a.i.?ha^?1 (recommended and double the recommended) in the dry and wet seasons under field conditions. Samples (green tea shoots, made tea, its infusion and spent leaves) were analysed for fenvalerate by high-performance liquid chromatography using diode array detection. The residue dissipated faster in the wet season than in the dry season. Seven days after the treatment (normal round of plucking) the residues observed in the green shoots at the two dosages were 0.5?±?0.01, 1.1?±?0.01 and 0.4?±?0.02, 0.9?±?0.01?mg?kg^?1 in the dry and wet seasons, respectively. During processing of green tea shoots to made tea a 30–40% loss of residue was observed. The transfer of residue from made tea to infusion was in the range 10–30% for both seasons, whereas 50–70% of the residues remained in the spent leaves. However, the degradation rate in both seasons followed first-order kinetics. The half-lives were in the range of 2–3 days for green shoots and made tea in both seasons.     

果蔬及其制品中真菌毒素的污染与检测研究进展

果蔬在生长、贮存、运输及加工等一系列过程中,极易受到各种病原菌的侵染而发生腐烂,腐烂果蔬不仅造成巨大的经济损失,而且导致果蔬积累大量的真菌毒素。真菌毒素可通过食物链的传递对人或动物的健康带来巨大威胁。本文就果蔬中常见真菌毒素的种类、产毒菌株、侵染途径、产毒条件、毒性作用、检测方法和限量标准等方面进行详细的总结,旨在为果蔬中真菌毒素的控制提供参考。     

蛋白质组学技术及其在乳及乳制品中的应用研究进展

蛋白质组学技术是近年来生命科学研究的重要工具,在食品、医学及动植物研究领域具有独特优势。利用蛋白质组学技术研究乳及乳制品,深入阐明其中蛋白质的表达及动态变化已成为当前的研究热点。该文主要综述了蛋白质组学的概念、常用技术及应用领域,重点介绍蛋白质组学在乳及乳制品领域,特别是在乳脂肪球膜蛋白、乳清蛋白、乳及乳制品加工过程以及干酪制品中的研究应用,探讨了目前乳及乳制品蛋白质组学研究中存在的问题与局限,并对蛋白质组学及其在乳及乳制品中的应用前景进行了总结与展望,为应用蛋白质组学技术深入研究乳及乳制品提供了理论依据。     

我国熟制坚果与籽类食品中霉菌及其毒素污染状况研究

目的 调查我国熟制坚果与籽类食品中霉菌及其毒素污染状况，掌握该类食品中霉菌及真菌毒素污染风险的关联性。方法 通过采集市售商品，检测霉菌及其毒素，采用内转录间区（ITS）测序法对样品中污染的霉菌进行属鉴定。结果 19.32%（560/2 912）的熟制坚果与籽类食品霉菌计数>25 CFU/g。单一、混合坚果超过该限值的比例分别为14.78%（322/2 178）和32.56%（239/734），差异有统计学意义（P<0.05）。单一坚果中核桃超过该限值的比例最高，为24.10%（47/195），杏仁、巴达木和花生分别为17.44%（15/86）、16.81%（20/119）和16.22%（73/450），其余种类均在15%以下。对26份霉菌计数>25 CFU/g的样品进行真菌毒素检测，1份采自云南的花生检出白僵菌素污染量为16.37 μg/kg。ITS扩增子测序发现熟制坚果与籽类食品中主要污染曲霉属、交链孢霉属、念珠菌属等，和真菌毒素检出有相关性。结论 熟制坚果与籽类食品中霉菌污染较高，检出的霉菌属有产真菌毒素的风险，提示应加强该类食品中污染霉菌的监测、种属鉴定及产毒情况研究，掌握其污染途径和产毒规律，为开展风险评估，采取有效防控措施提供科学依据。     

冰酒中的毕赤属和汉逊属酵母菌的筛选及其在葡萄酒酿造中的应用

从冰葡萄酒自然发酵过程中分离、鉴定出10株毕赤属(Pichia)和汉逊属(Hanseniaspora)酵母,对其耐受性(酒精、糖、酸、SO2)进行研究,筛选得到4株耐受性能优良的酵母菌株,编号为"HO"和"HU"(Hanseniaspora属)、"PO"和"PK"(Pichia属).再将此4个酵母菌株与商业酿酒酵母(S...     

Sweetness and aroma perceptions in dairy desserts varying in sucrose and aroma levels and in textural agent

Sweetness–aroma interactions were investigated in model dairy desserts varying in sucrose concentration, aroma concentration and in textural characteristics using different textural agents (κ-, ι-, λ-carrageenans and an equal-mix of the three). Overall intensities of sweetness and aroma perceptions were evaluated by sensory analysis and apparent partition coefficients of aroma compounds were measured by static headspace—GC.Sweetness–aroma interaction was characterised by a non-reciprocal relationship. Concentration of aroma had no impact on sweetness intensity, whatever be the sucrose concentration or textural characteristics of desserts, whereas varying texture or sucrose concentration modified aroma intensity. However, effects on aroma assessment were effective only when aroma concentration was the highest. In this condition, use of λ-carrageenan or increasing sucrose concentration from 25 to 50 g kg⁻¹ enhanced aroma intensity, but no extra enhancement was observed when sucrose concentration was 100 g kg⁻¹. As the air–dessert partition coefficient remained constant, impact of textural characteristics and sweetness variation on aroma perception did not result from physico-chemical interaction.     

Fenvalerate residue level and dissipation in tea and in its infusion

Fenvalerate is a non-systemic insecticide/acaricide used in controlling a wide range of pests, including those resistant to organochlorine, organophosphorus and carbamate insecticides. The study investigated the dissipation behaviour (residue level) of fenvalerate in tea and its transfer during infusion. Fenvalerate was applied on tea crop at two dosages, 100 and 200 g a.i. ha^-1 (recommended and double the recommended) in the dry and wet seasons under field conditions. Samples (green tea shoots, made tea, its infusion and spent leaves) were analysed for fenvalerate by high-performance liquid chromatography using diode array detection. The residue dissipated faster in the wet season than in the dry season. Seven days after the treatment (normal round of plucking) the residues observed in the green shoots at the two dosages were 0.5 ± 0.01, 1.1 ± 0.01 and 0.4 ± 0.02, 0.9 ± 0.01 mg kg^-1 in the dry and wet seasons, respectively. During processing of green tea shoots to made tea a 30-40% loss of residue was observed. The transfer of residue from made tea to infusion was in the range 10-30% for both seasons, whereas 50-70% of the residues remained in the spent leaves. However, the degradation rate in both seasons followed first-order kinetics. The half-lives were in the range of 2-3 days for green shoots and made tea in both seasons.