基于液相色谱-串联质谱法的纺织品中痕量全氟化合物的测定

采用超声法提取纺织品中的全氟化合物。以C18为分析柱,甲醇-5 mmol/L乙酸铵为梯度洗脱淋洗液, 13 min内即可分离全氟己酸(PFHxA),全氟辛酸(PFOA),全氟壬酸(PFNA),全氟癸酸(PFDA),全氟十一酸(PFuDA),全氟十二酸(PFDoA), 全氟丁烷磺酸(PFBS),全氟己烷磺酸(PFHxS),全氟辛烷磺酸(PFOS),全氟癸烷磺酸(PFDS) 10种分析物。以313.1/268.9,412.9/368.9,462.9/418.9,512.7/468.9,562.7/518.9,612.8/568.9,298.8/99,399.2/99,498.8/99,599/99分别对PFHxA,PFOA,PFNA,PFDA,PFuDA,PFDoA,PFBS,PFHxS,PFOS,PFDS进行监控和定量分析。利用同位素内标法进行定量,线性范围和添加回收率分别为0.5～10 µg/m2、84.6%～111.8%,检出限为0.5 µg/m2,低于欧盟指定针对纺织品1 µg/m2 的限定。结果表明,本方法准确、快速,并成功用于20种纺织品实样的检测。     

广东省典型氟化工区周边蔬菜中3种全氟化合物及2种氯代多氟醚基磺酸的污染调查及膳食暴露评估

目的 调查分析广东省典型氟化工区周边种植的蔬菜中3种全氟化合物及2种氯代多氟醚基磺酸的污染现状及膳食暴露风险。方法 2019年在广东省3个氟化工区周边随机采集种植蔬菜及非氟化工区农贸市场市售样品共96份,采用同位素稀释超高效液相色谱-三重四级杆质谱法检测样品中全氟辛烷磺酸（PFOS）、全氟辛酸（PFOA）、全氟己烷磺酸（PFHxS）、6：2氯代多氟醚基磺酸（6：2 Cl-PFESA）和8：2氯代多氟醚基磺酸（8：2 Cl-PFESA）的浓度,并采用点评估法对食用蔬菜暴露5种化合物的健康风险进行评估。结果 所有样品均检出PFOS和PFOA,仅在2份叶类蔬菜检出氯代多氟醚基磺酸。样品中5种化合物的平均浓度之和（∑₃ PFASs+∑₂ Cl-PFESA）为0.792 ng/g fw （fresh weight,鲜质量）,其中氟化工区周边样品的平均浓度为农贸市场市售样品的2倍。在3类蔬菜样品中,叶类蔬菜5种化合物的平均浓度之和最高,为1.11 ng/g fw。暴露评估结果显示,通过食用氟化工区周边种植的蔬菜暴露PFOS、PFOA和PFHxS的范围为0.185~2.35 ng/kg·BW,其中PFOS和PFOA的危害指数（HI）大于1,2种氯代多氟醚基磺酸的暴露水平较低。结论 居民食用氟化工区周边种植的叶类和瓜果类蔬菜暴露PFOS和PFOA的水平已超过健康指导值,存在潜在健康风险。经蔬菜暴露2种氯代多氟醚基磺酸的健康风险较低,但仍需关注。     

全氟辛烷磺酸、全氟辛酸及其盐类检验技术的研究进展

全氟辛烷磺酸(PFOS)、全氟辛酸(PFOA)及其盐类物质具有生殖毒性、诱变毒性和发育毒性等多种毒性,也是目前最难降解的持久性有机污染物.全氟化合物独特的拒水拒油性,使其被广泛地应用于纺织、皮革、造纸等行业.PFOS和PFOA及其盐类物质通过食品包装材料,已经不知不觉进入我们的食品中,影响了食品安全,威胁着人们的身体健...     

北京市场食用油中全氟化合物污染调查及其膳食风险评估

研究了北京市市售植物性油脂中全氟化合物的污染水平,测定了4个超市中大豆油、花生油、芝麻油等6类植物油中18种全氟化合物,结果表明:北京市售植物性油脂中均存在一定浓度的全氟化合物污染,其中品牌油脂中共检出8种全氟化合物,以全氟辛酸(PFOA)、全氟壬酸(PFNA)和全氟己酸(PFHxA)为主,其中调和油中的PFNA最高浓度达到4.64μg/kg,而在油作坊采集的压榨油脂中共检出15种全氟化合物,浓度均较品牌油脂高,其安全问题值得关注。对植物性油脂中全氟化合物的膳食风险评估结果显示,北京市售植物性油脂产品中PFOS和PFOA的污染水平和膳食暴露均在可接受的范围内。     

纺织品中全氟辛烷磺酸及全氟辛酸的测定及其研究进展

全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)等化合物是应用广泛但对环境有持久污染的有机物.开展纺织品中PFOS和PFOA检测方法的研究是保护环境和人类健康,提升纺织产品质量的迫切要求.简述了PFOS和PFOA的各种检测方法和复杂样品的前处理技术,指出应研究有关纺织品中PFOS和PFOA快速、精确的测定方法,并尽快建立...     

液相色谱-串联质谱法测定上光剂中全氟化合物

建立了针对上光剂中包括全氟己酸(PFHx A)、全氟辛酸(PFOA)、全氟壬酸(PFNA)、全氟癸酸(PFDA)、全氟十一酸(PFu DA)、全氟十二酸(PFDo A)、全氟丁烷磺酸(PFBS)、全氟己烷磺酸(PFHx S)、全氟辛烷磺酸(PFOS)、全氟癸烷磺酸(PFDS)在内的10种全氟化合物(PFCs)的液相色谱-串联质谱法(LC-MS/MS)测定分析方法。采用超声法提取测试目标化合物,提取液用混合型弱阴离子交换固相萃取柱净化,用液相色谱-串联质谱仪测定。结果表明,该方法的检测低限均为50μg/kg,相对标准偏差在10%以内,加标回收率85.5%~106.0%。该方法准确、快速,能满足上光剂中全氟化合物测定要求。     

制革行业中的全氟化合物及其检测

简单介绍了全氟化合物及其潜在的环境风险,概述了全氟化合物在制革工业中的应用,并对全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的分析检测方法进展进行了归纳和总结。     

食品接触材料中全氟化合物检测方法的研究进展

全氟化合物主要包括全氟辛酸(PFOA)、全氟辛烷磺酸(PFOS) 及其盐类物质, 是目前最难降解的持久性有机污染物之一。全氟化合物具有高效的疏水和疏油特性, 因此被广泛地应用于纺织、造纸、皮革等行业。然而其具有生殖毒性、遗传毒性和发育毒性等多种毒性, 可以通过食品接触材料进入人们的食品中, 威胁着人们的身体健康。本文简述了全氟化合物的概况及其在食品接触材料中分析检测技术的研究进展。     

14种新污染物于3月1日起重点管控，包括全氟辛基磺酰氟（PFOS类）

<正>生态环境部等六部门公布的《重点管控新污染物清单（2023年版）》，于2023年3月1日起施行。清单内以下14类新污染物：全氟辛基磺酸及其盐类和全氟辛基磺酰氟（PFOS类）；全氟辛酸及其盐类和相关化合物（PFOA类）；十溴二苯醚；短链氯化石蜡；六氯丁二烯；五氯苯酚及其盐类和酯类；三氯杀螨醇；全氟己基磺酸及其盐类和其相关化合物（PFHx S类）；得克隆及其顺式异构体和反式异构体；     

中国部分主产区鸡肉中全氟化合物残留水平调查

目的通过对中国鸡肉部分主产区2014年1月至2015年4月的619份鸡肉样品中19种全氟化合物(11种全氟羧酸和8种全氟磺酸盐)浓度的检测,进行全氟化合物在鸡肉中污染状况的分析评价。方法样品采用溶剂萃取固相填料净化结合高效液相色谱-串联质谱法(HPLC-MS/MS)进行分析。结果 619份鸡肉样品中全氟化合物的总检出率为83.8%,共检出17种全氟化合物,以全氟戊酸(perfluoropentanoic acid,PFPe A)、全氟辛酸(perfluorooctanoic acid,PFOA)和全氟壬酸(perfluorononanoic acid,PFNA)的残留为主,其含量分别为0~1.26μg/kg,0~2.19μg/kg和0~0.76μg/kg。结论鸡肉部分主产区中PFCs的残留水平具有区域差异,人体健康风险评价表明,该4省市的鸡肉中PFOA和全氟辛烷磺酸盐(PFOS)不会对人体造成即时危害。     

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.     

2018年深圳市售蔬菜和鸡蛋中氟虫腈及其代谢物的检测分析

目的 建立超高效液相色谱-串联质谱法同时测定蔬菜和鸡蛋中氟虫腈及其代谢物(氟甲腈、氟虫腈砜和氟虫腈亚砜), 并对深圳市售的蔬菜和鸡蛋中氟虫腈及其代谢物残留状况进行抽样检测。方法 采用QuEChERS前处理方法, 以C18色谱柱为分离柱, 以乙腈和10 mmol甲酸+6 mmol甲酸铵水溶液为流动相进行梯度洗脱, 用超高效液相色谱-串联质谱(ultra performance liquid chromatography-mass spectrometry/mass spectrometry, UPLC-MS/MS), 电喷雾电离(electrospray ionization, ESI), 多反应监测(multiple reaction monitoring, MRM)模式检测, 外标法同时定量测定氟虫腈及其代谢物。结果 方法的线性范围为0.1~2.0 μg/L, 线性相关系数均大于0.9994, 检出限0.0005 mg/kg, 定量限0.001 mg/kg; 蔬菜中3个水平的平均加标回收率88.0%~101.2%, 相对标准偏差(relative standard deviation, RSD)均小于8.5%; 鸡蛋中3个水平的平均加标回收率86.1%~104.8%, 相对标准偏差(RSD)均小于9.2%。结论 该方法具有操作简单、干扰少、快速、准确可靠等特点, 可适用于蔬菜鸡蛋中氟虫腈及其代谢物的检测。     

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.     

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。     

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(Saccharomyces cerevisiae)按不同比例(1:1和10:1,1:1编号为1,10:1编号为2),先接种非酿酒酵母菌株,48 h后再接种酿酒酵母的顺序进行混合发酵。研究了发酵过程中菌群及乙醇的动态变化,又对发酵结束后冰葡萄酒的主要成分进行分析。结果显示:"HO"随接种量的增加菌落数受到抑制,"HU""PO"及"PK"随接种量的增大菌落数受到促进作用;HO1、HU1、HU2、PK1、PK2乙醇含量在发酵前期增长较少,在发酵中期迅速增大,HO2、PO1、PO2乙醇含量在发酵前期增长较多,在发酵中期显著增大,所有发酵乙醇含量皆于第21天稳定在9%左右;"HO""HU""PO"及"PK"不同比例混合发酵各理化指标(酒精度、总糖、总酸、有机酸)均符合国家葡萄酒标准,"HU"乙酸含量过高,葡萄酒品质中含有缺陷。以上结果表明4株酵母菌株均可应用于本土葡萄酒的酿造中,为生产具有本地特色的葡萄酒提供一定的参考。     

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.     

生物技术在制浆造纸中的应用与研究进展

介绍了生物技术在制浆造纸工业的应用与研究进展，包括生物制浆、生物漂白、生物脱墨及造纸过程中的生物技术等。     

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.