电感耦合等离子发射光谱法测定铅法皮蛋中的多种无机元素含量

采用电感耦合等离子发射光谱法(ICP-AES)对鲜鸭蛋和铅法皮蛋蛋壳、蛋白、蛋黄中的Pb、Cu、Mg、Zn、Ca、Fe 等20 种无机元素进行分析测定。该方法的加标回收率为84.4%～112.2%,相对标准偏差小于7%,20 种元素的方法检测限在0.4～10g/L 之间。结果表明：铅法皮蛋可食部分中富含多种人体所必需的无机元素,且其蛋黄中的大部分有机元素含量皆高于蛋白。鲜鸭蛋经加工成皮蛋后,Cu、Fe、Al、Pb、Mn 等元素在各部位含量明显升高,其中有害元素Pb 的含量大大提高,且由外到内其Pb 的含量增幅呈逐渐减少的趋势。实验同时说明：ICP-AES 法是一种快速、准确、灵敏测定皮蛋中无机元素的有效方法。     

金属盐对清料法腌制皮蛋品质的影响

以鸭蛋为原料,通过比较不同金属盐清料法加工的皮蛋的安全性能和感官性质,研究了金属盐的种类和添加量对皮蛋品质的影响。试验结果表明:分别添加了Cu SO4、Cu SO4:Zn SO4=1:1和Zn SO4:Fe SO4=1:1腌制的皮蛋的感官品质都较好,评分分别为90.60±2.40、89.80±3.20、88.20±2.70;添加了Zn SO4溶液次之,感官评分为85.80±3.80;单独添加Fe SO4、Mg SO4盐腌制的皮蛋感官品质比较低;添加Cu SO4:Zn SO4=1:1的溶液腌制的皮蛋,锌铜的残留量(铜离子4.12±0.11 mg/kg,锌离子8.32±0.19 mg/kg)比显著低于分别添加锌盐(12.96±0.22 mg/kg)和铜盐(铜离子8.55±0.28 mg/kg)的低皮蛋(P0.05);不同锌盐对皮蛋感官品质的影响有区别,用氧化锌生产的皮蛋锌的残留量(9.27±0.09 mg/kg)和感官评分显著低于其他锌盐腌制的皮蛋,综合考虑,Zn SO4是腌制皮蛋较适合的锌盐;添加Cu SO4或Cu SO4:Zn SO4=1:1生产的皮蛋,蛋黄的溏心指数较高(0.66、0.57),皮蛋的弹性、硬度、咀嚼度较好,因此,从感官品质和金属的残留量两方面考虑,用Cu SO4和Zn SO4混合清料法腌制皮蛋比较好,而单独添加Fe SO4生产皮蛋明显不适合。     

Cadmium,lead and some other trace elements in Larch Bolete mushrooms (Suillus grevillei) (Klotzsch) Sing., collected from the same site over two years

The aim of this study was to examine the status of some trace metals accumulated in the flesh of Suillus grevillei mushrooms collected from the same site over two successive years. Total Ag, Al, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, Pb, Rb, Sr and Zn contents of fruiting bodies were determined by inductively coupled plasma atomic emission spectroscopy (ICP-AES) with ultrasonic cross-flow nebuliser. A difference (p < 0.05) was found in the contents of Cd, Cr, Cu, Fe, K, Na, Ni, Pb, Rb and Sr in caps and Fe, Na, P and Rb (p < 0.05) in stipes (Ag, Cd, Co, Cr, Ni and Pb were not determined in stipes). Natural fluctuations in trace elements’ content of Suillus grevillei collected from the same site over time is a variable that needs to be considered when assessing minerals’ nutritional status of mushrooms.     

皮蛋壳表层红色斑块成分的分析与鉴定

目的 分析鉴定皮蛋壳表面红色斑块物质组成成分, 为控制红斑生成提供理论依据。方法 采用场发射扫描电镜(Scanning Electron Microscope, SEM)、X射线衍射仪(X-ray Diffractometer, XRD)、X射线电子能谱仪(X-ray Photo-electron Spectroscopy, XPS)分析皮蛋壳表面红色斑块的微观结构和化学成分。结果 皮蛋壳表面红色斑块物质是大块片状物附着在粗糙的碳酸钙晶体外层, 蛋壳气孔也被块状异物堵塞, XPS检测出红斑由C、O、N、Na、Ca、Fe、Cu、S、Zn、P等元素组成, Fe元素含量低, 未检出Pb元素; XRD分析确定红斑的主要物质是Cu2O, 红斑外层Cu+因氧化而成Cu2+。结论 皮蛋壳表面红色斑块主成分为Cu2O。采取鸭蛋消毒控菌, 低温避光腌制或许可控制蛋壳红斑形成。     

ICP-AES法测定小米和高粱米中的金属元素

用微波消解,电感耦合等离子体发射光谱法测定小米和高粱米中的金属元素。试验结果表明,2种粗粮中富含多种对人体有益的K,Na、Ca、Mg、Al、Fe、Zn、Cu等金属元素。对比发现,高粱米中各种金属元素的含量远远超过大米,8种金属元素的含量均是大米的几十至几百倍;小米中的各种金属元素的含量也超过大米。可见小米和高粱米是人们饮食中很好的矿物质来源。方法回收率在92.0%～102.0%之间,相对标准偏差小于4.8%。方法操作简单,分析速度快,准确度高,灵敏度好。     

贵州三穗特色黄皮蛋无铅腌制过程中色泽及蛋黄凝固度变化分析

为了探究无铅腌制过程中皮蛋色泽及蛋黄凝固度变化,以黄皮蛋无铅腌制工艺为基础,用硫酸铜与硫酸锌复配剂代替氧化铅,探究铜锌复配液浓度、铜锌复配比、腌制温度、Na OH浓度、腌制时间对皮蛋色泽、蛋黄凝固度的影响。结果表明:腌制温度、Na OH浓度和腌制时间为主要影响因素,并在主要因素的研究基础上得到皮蛋色泽、蛋黄凝固度以及感官品质最佳的特色黄皮蛋腌制条件为:铜锌复配液浓度0.40%、铜锌复配比为1:2、腌制温度15℃、Na OH浓度4%、腌制时间18 d。该腌制条件下,皮蛋的蛋黄凝固度为0.85、蛋清白度值(w)为30.15、蛋黄白度值(w)为46.72,此时皮蛋呈半透明的黄色、凝胶完整、软硬适中、具有光泽性。皮蛋品质优秀,感官评分为81.35、综合评分为0.92。综上所述,该研究为无铅腌制皮蛋的生产提供了理论基础。     

绿豆、红小豆和黑豆种皮18 种元素分析

为全面了解绿豆皮、红小豆皮和黑豆皮的18 种元素含量,充分开发利用豆皮资源,提高豆类加工产品
的附加值,用元素分析（elemental analyzer,EA）仪和电感耦合等离子体发射光谱（inductively coupled plasmaatomic
emission spectrometer,ICP-AES）仪测定了3 种豆皮的N、C、S、Ca、Mg、K、P、Na、B、Ba、Co、
Cr、Cu、Fe、Mn、Ni、Zn和Sr元素含量。结果表明,EA仪测定豆皮中N、C和S方法检出限为32～96 μg/g,回收
率为97%～115%,相对标准偏差为0.20%～2.63%（n=5）;ICP-AES测定豆皮中Ca、Mg、K、P、Na、B、Ba、
Co、Cr、Cu、Fe、Mn、Ni、Zn和Sr元素方法检出限为0.02～152 μg/g,回收率为84%～118%,相对标准偏差为
0.44%～4.46%（n=5）。黄豆标准物N、Mg、P、B、Ba、Co、Cr、Mn、Ni、Zn和Sr元素测定值在推荐范围内,
S、Ca、K、Na、Cu和Fe元素测定值接近推荐值。分析方法快速、简便,达到了应用的要求。     

Doxycycline depletion and residues in eggs after oral administration to laying hens

The depletion of doxycycline (DC) residues in eggs was determined after oral drug administration by drinking water to laying hens. The antibiotic was supplied to birds for 5 consecutive days and the eggs were collected during medication and 18 days after withdrawal. DC residues were determined by LC-MS/MS. DC was isolated from eggs with a solution of 0.02 M of oxalic acid (pH 4), 0.1 M Na₂EDTA and acetonitrile. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 2 and 5 µg kg^–1, respectively. Analyses were performed on whole egg, egg white and yolk separately. DC was detectable 24 h after the beginning of administration. The concentration of antibiotic increased daily, resulting in the highest DC concentration in whole eggs at the first day of the withdrawal period. Thirteen days after withdrawal, the content of DC in whole eggs was below the LOQ of the method. However, some differences were found in the depletion curve of DC between egg white and yolk. Residues of DC in egg white were much higher during treatment and 1 day after withdrawal, but later the concentration in egg white decreased fairly rapidly and a higher DC content in egg yolk was observed. The depletion period was shorter for egg white than for yolk, and DC was detected in the egg white until 12 days after withdrawal and 2 days more in egg yolk than in white. DC reached a peak faster in egg white, but the residues were detectable for longer period in the yolk.     

加丽素红在市售鸡蛋中残留情况的研究

目的:加丽素红是一种化学合成类饲料着色剂,主要用于改善家禽皮肤、蛋黄等组织的色泽,被广泛应用在动物养殖业中。本研究为了解饲用着色剂加丽素红在鸡蛋中的残留情况而开展的。方法:以昆明市场上的鲜鸡蛋为研究对象,利用高效液相色谱法对市售鲜鸡蛋中是否含有加丽素红及其含量多少进行研究。结果:64份市售鸡蛋样品中,检出含有加丽素红的样品23份、未检出41份,总体阳性检出率为35.94%;检出的样品中含有加丽素红,含量范围为7.37μg/g≦C≦91.3μg/g,平均值为33.3μg/g。结论:云南省鸡蛋市场上确实有加丽素红残留的鸡蛋存在,且由于鸡蛋品种、来源的不同,加丽素红含量水平有一定差异。     

新疆6种辣椒籽中矿质元素测定及聚类分析

目的：分析不同品种辣椒籽中的矿质元素含量,并进行聚类分析,评价其营养价值。方法：采用电感耦合等离子体发射光谱(inductively coupled plasma-atomic emission spectrometry,ICP-AES)法测定Zn、Cu、Fe、Mn、Ca、Mg、Na、K。结果：辣椒籽中富含多种矿质元素,常量元素K/Na、Mg/Na比值高,微量元素Fe含量最为丰富,Zn、Cu含量相对较少,Zn/Cu比值在2.01～1.36之间;从元素含量的角度进行聚类分析,6个辣椒籽品种可以分为两大类。结论：辣椒籽中矿质元素含量高,具有食品开发的价值。     

微波密闭消解-ICP-AES同时测定贼小豆中18 种矿物质元素

为探讨郑州地区野生贼小豆中微量元素的组成、含量和分布特性,充分开发利用贼小豆自然资源,用微波 密闭消解-电感耦合等离子体发射光谱法同时测定了贼小豆样品中Al、Ba、Ca、Cd、Co、Cr、Cu、Fe、Hg等18 种 微量元素。结果表明：在优化条件下,待测各元素间相互干扰较小,18种元素在一定范围具有良好的线性关系,相 关系数（r）均不小于0.995 0,检出限范围为0.000 1～0.035 μg/mL,定量限范围为0.000 17～0.058 μg/mL,平均回收率 为97.08%～113.06%,相对标准偏差为0.14%～3.2%（n=6）。该法所用样品和消解剂量少,消解完全、快速省时,待 测元素不易挥发损失,可同时测定18 种矿物质元素,工作效率较高,用于贼小豆样品的测定,结果令人满意。     

西青果中化学元素的测定研究

西青果样品经微波消解后,以ICP-MS/ICP-AES法联合测定其中的24种元素,方法的准确性用国家一级标准物质GBW10015、GBW10020进行对归照分析。检测结果显示,本方法检出限低,准确度高,精密度好,完全可以满足样品中元素含量测定要求。从检测结果来看西青果中富含K、Mg、Ca、P等宏量元素及Fe、Zn、Mn、Cu等微量元素,其中K含量最高为11100μg/g,而Be、Cd、Mo、Tl含量较低,均低于0.3μg/g。所测定元素的含量顺序依次为K>Ca>Mg>P>Al>Fe>Ti>B>Na>Zn>Mn>Cu>Sr>Ba>Ni>V>Cr>Pb>Co>Li>Mo>Cd>Be>Tl。     

ICP-AES法测定葡萄干中常微量元素含量

分别采用湿法、微波消解法处理样品,以电感耦合等离子体发射光谱仪(ICP-AES)检测不同等级的新疆吐鲁番葡萄干中Cu、Fe、Zn、Mn、Na、K、Ca、Mg、P等9种元素的含量,并优化微波处理样品条件。结果表明:葡萄干中Fe、Na、K、Ca、Mg、P等元素的含量较高,ICP-AES检测各元素的相对标准偏差为0.01%～4.90%,各元素回收率在98.15%～102.13%。无论湿法还是微波法消化样品,测定结果基本一致。采用微波消解技术和ICP-AES法结合测定常微量元素具有省时、省力、环境污染小,测定结果快速、准确等优点。     

Micronutrients (B,Co, Cu,Fe, Mn,Mo, and Zn) content in made tea (Camellia sinensis L.) and tea infusion with health prospect: A critical review

Tea (Camellia sinensis L.) is a perennial acidophilic crop, and known to be a nonalcoholic stimulating beverage that is most widely consumed after water. The aim of this review paper is to provide a detailed documentation of selected micronutrient contents, viz. boron (B), cobalt (Co), copper (Cu), iron (Fe), manganese (Mn), molybdenum (Mo), and zinc (Zn) in made tea and tea infusion. Available data from the literature were used to calculate human health aspect associated with the consumption of tea infusion. A wide range of micronutrients reported in both made tea and tea infusion could be the major sources of micronutrients for human. The content of B, Co, Cu, Fe, Mn, Mo, and Zn in made tea are ranged from 3.04 to 58.44 μg g^?1, below detectable limit (BDL) to 122.4 μg g^?1, BDL to 602 μg g^?1, 0.275 to 13,040 μg g^?1, 0.004 to 15,866 μg g^?1, 0.04 to 570.80 μg g^?1 and 0.01 to 1120 μg g^?1, respectively. Only 3.2 μg L^?1 to 7.25 mg L^?1, 0.01 μg L^?1 to 7 mg L^?1, 3.80 μg L^?1 to 6.13 mg L^?1, 135.59 μg L^?1 ?11.05 mg L^?1, 0.05 μg L^?1 to 1980.34 mg L^?1, 0.012 to 3.78 μg L^?1, and 1.12 μg L^?1 to 2.32 μg L^?1 of B, Co, Cu, Fe, Mn, Mo, and Zn, respectively, are found in tea infusion which are lower than the prescribed limit of micronutrients in drinking water by World Health Organization. Furthermore, micronutrient contents in tea infusion depend on infusion procedure as well as on the instrument used for analysis. The proportion of micronutrients found in different tea types are 1.0–88.9% for B, 10–60% for Co, 2.0–97.8% for Cu, 67.8–89.9% for Fe, 71.0–87.4% for Mn, 13.3–34% for Mo, and 34.9–83% for Zn. From the results, it can also be concluded that consumption of three cups of tea infusion per day does not have any adverse effect on human health with respect to the referred micronutrients rather got beneficial effects to human.     

沙棘果油脂肪酸与微量元素测定

该文测定了沙棘果油中脂肪酸与8种微量元素。沙棘果油由亚临界流体萃取而得,经脂肪皂化和脂肪酸甲酯化,气相色谱-质谱联用法测定脂肪酸,内标法定量;在浓HNO 3中经微波消解,电感耦合等离子体原子发射光谱法测定微量元素,外标法定量。共检测到19种脂肪酸,其中饱和脂肪酸、单不饱和脂肪酸、多不饱和脂肪酸百分比含量分别为24.42%、47.26%和28.31%,C16∶0、C16∶1、C18∶1、C18∶2、C18∶3含量较高,分别为39.71、44.29、48.15、35.25和35.25 mg/g。试样中K、Na、Ca、Mg、Cu、Zn、Fe和Mn的检测限分别为0.5、0.25、0.125、0.1、0.1、0.1、0.2和0.4μg/g,各元素的平均回收率为85.0%~94.4%,相对标准偏差(relative standard deviation,RSD)为3.28%~9.23%(RSD<10%)。沙棘果油中Na、Ca、K、Mg、Fe、Zn含量较高,分别为149.28、65.29、41.08、21.27、14.43和4.71μg/g。沙棘果油中不饱和脂肪酸与人体所需微量元素含量较高,具有很高的营养价值,该研究结果为沙棘的进一步开发利用提供了基础数据。     

腌制剂及复配对无重金属盐皮蛋品质的影响

为解决无重金属盐皮蛋易出现的“碱伤”、“烂头”等问题,改善无重金属盐皮蛋品质,本研究以鸡蛋为原料,采用清料法腌制皮蛋,加入葡萄糖、单宁、葡萄糖酸-δ-内酯三种非金属腌制剂,通过单因素实验选择最佳添加量,之后进行复配,以蛋清硬度、游离碱度、色度以及蛋黄硬化率为指标,结合腌制20 d皮蛋的感官评价及蛋壳微观结构,考察各复配组对皮蛋品质的影响。结果表明:单独添加0.7%葡萄糖、0.5%单宁、0.7%葡萄糖酸-δ-内酯腌制组皮蛋碱伤程度均有所改善,其中0.7%葡萄糖酸-δ-内酯改腌制组改善效果最好。最优复配组为0.7%葡萄糖+0.7%葡萄糖酸-δ-内酯,腌制20 d,皮蛋蛋黄硬化率为86.69%,蛋清硬度值为183.584 g,蛋清游离碱度为240.371 mg/100 g,色泽为深红棕色,感官品质最好,未出现“碱伤”和“烂头”的现象。     

Depletion of florfenicol and florfenicol amine in eggs of laying hens and growing pullets after oral administration

ABSTRACT

In this study, we carried out two experiments to evaluate depletion of florfenicol (FF) and its metabolite florfenicol amine (FFA) in eggs from growing pullets and laying hens. Eggs were collected, and the egg white and yolk were separated. FF and FFA were analysed by liquid chromatography-tandem mass spectrometry. In the first experiment, 30 laying hens were given FF capsules at 50 mg/kg·bw^?1 daily for 5 d. FF + FFA was detectable in egg white (1,190 µg/kg) on day 1 of treatment and increased slowly thereafter. After treatment, the residues decreased rapidly and were not detected by day 11. In yolk, residues were detected at a lower concentration on day 1 and increased dramatically to 3308 µg/kg at the end of treatment. The residues remained steady over the next 4 days post-treatment, followed by a rapid drop. Residues were not detectable on day 15 post-treatment. In the second experiment, four groups (B1 through B4) of growing pullets were treated in the same manner for 25, 20, 15, and 10 days before egg primiparity. FF and FFA were not detectable in the eggs of group B1; however, they were detectable in egg whites and yolks of groups B2, B3, and B4. The highest total concentrations of FF and FFA detected in egg white and yolk of group B4 were 3,190 µg/kg and 3,214 µg/kg, respectively. Thereafter, concentrations decreased until no more residues were detected in egg whites or yolks on days 17 and 21 post-treatment, respectively. Therefore, drug treatment should be stopped at least 21 d before primiparity of growing pullets to guarantee food safety.     

ICP-AES法测定水产品贝壳肉中16种金属元素

利用ICP-AES法测定钱塘江近海水域水产品贝壳肉中Al、Ca、Cr、Cu、Fe、Mg、Mn、Ni、Se、Sb、Sn、V 、Zn、Cd、As、Pb、Hg十六种金属元素含量。结果表明:所采样品金属元素含量丰富,对铅、铝的吸附量相对较高,部分样品金属元素含量相对偏高,不宜多食。ICP-AES法具有检测灵敏度高、回收率好、快速、简便等好的检测效果。     

西施舌可食部分微量元素分析与评价

分析西施舌可食部分不同部位微量元素含量,评价其营养价值和重金属污染情况。用硝酸-高氯酸消化法消解组织,用电感耦合等离子体发射光谱(inductively coupled plasma atomic emission spectrometry technique,ICP-AES)法测定黄海日照、东海漳州、北部湾越南某海区(毗邻广西北海)3个地区西施舌闭壳肌、外套膜、斧足、鳃、内脏团5个部位(组织/器官)的12种元素。比较Ag、As、Cd、Co、Cr、Cu、Fe、Mn、Pb、Se、Sn、Zn元素在不同地域和不同部位的分布和含量。结果显示：10种元素的加标回收率为78.3%～112.1%,相对标准偏差为0.16%～7.46%;西施舌富含Fe、Zn、Mn、Cu、Se等人体必需的微量元素,Ag和Sn元素含量低;多数元素在同域不同部位的含量存在显著差异(P＜0.05),日照西施舌外套膜、内脏团Fe的含量显著(P＜0.05)高于同域其他组织及漳州、越南西施舌所有组织;西施舌As、Cd的含量超过国家卫生限量标准,但Cd的含量低于世界卫生组织、澳大利亚、香港的限量标准。     

火焰原子吸收法测定马齿苋中10种无机元素

目的测定马齿苋中无机元素含量,为其药效学研究及食用开发提供资料。方法利用火焰原子吸收光谱法测定马齿苋中钾、钙、钠、镁、铜、锌、铁、锰、铬、镍的含量。结果马齿苋所含10种无机元素中,钾、钙、镁为宏量元素,其余7种为微量元素。结论本研究为马齿苋的后续研究及进一步开发应用提供数据支持。