母乳与牛乳中微量元素的比较

用ＩＣＰ－ＡＥＳ法对母乳和牛乳中Ｋ、Ｎａ、Ｃａ、Ｍｇ、Ｐ、Ｆｅ、Ａｌ、Ｚｎ、Ｓｒ、、Ｐｂ、Ｍｎ、Ｂａ和Ｃｕ等１３种元素含量进行了测定。结果发现母乳与牛乳的营养成分差异较大。研究了深入探讨微量元素在人体内重要的生理功能提供了有用的参考数据。     

广州某黑臭河涌沉积物中的挥发物质组分

在广州市城区内的猎德涌采集了3个采样点中0~10cm深的表层沉积物,通过DVB/CAR/PDMS固相微萃取(SPME)纤维顶空富集,使用气相色谱/质谱联用仪(GC/MS)对其挥发物进行检测分析。在猎德涌的沉积物中共检测出54种挥发物质,包括36种烷烃、2种环烷烃、1种烯烃、2种硫单体、13种带有发香基团的有机物。在3个采样点分别鉴定出19、49、52种挥发物。在下游河段沉积物中检测出的挥发物种类和峰面积都超过上游。由挥发物质的组成可以判断出其主要污染是来源于交通污染和居民的日常生活污染,其中有3种毒性较大的成分:万山麝香、邻苯二甲酸二异丁酯(DIBP)和2,4-二叔丁基苯酚。     

沉淀分离富集-电感耦合等离子原子发射光谱测定土壤中可溶态稀土元素

研究电感耦合等离子体原子发射光谱测定土壤中微量可溶态稀土元素的方法。在适宜的ｐＨ＝１０－１１条件下,以ＭｇＣｌ２为载体沉淀分离除去浸提液中的大部分基体杂质如Ｎａ＾＋,Ａｃ＾－,Ｃａ＾２＋,Ｍｇ＾２＋等,有效地消除了这些杂质的干扰,提高了测定方法的准确度;同时,待测可溶态稀土元素被沉淀集,样品中总稀土及单一稀土加标回收率为８８％－１１０％,样品测定结果满意,方法简便快速。     

LC-MS/MS法测定沉积物中磺胺类和四环素类抗生素

沉积物样品用乙腈-柠檬酸缓冲溶液提取后经HLB-SPE柱净化,采用LC-MS/MS法在MRM模式下测定17种磺胺类和4种四环素类抗生素,通过优化测定条件,使方法在0. 500μg/kg～100μg/kg范围内线性良好。方法检出限为0. 15μg/kg～1. 2μg/kg,2个质量比水平的加标回收率为44. 1%～125%,试验5次结果的RSD 16. 0%。将该方法用于测定厦门近岸海域沉积物中抗生素,共有6种磺胺类和4种四环素类抗生素检出,测定值为0. 3μg/kg～26. 2μg/kg。     

UPLC-串联质谱法快速测定地表水中多种农药残留

采用超高效液相色谱-串联质谱法测定地表水中21种氨基甲酸酯和有机磷农药,通过优化试验条件,使方法在0. 500μg/L～100μg/L范围内线性良好,方法检出限为0. 1μg/L～6. 2μg/L。对空白水样做3个质量浓度水平的加标回收试验,5次测定结果的RSD为0. 3%～9. 5%,回收率为82. 0%～113%。将该方法用于测定徐州某地表水样品,3个水样均为未检出。     

UPLC-MS/MS法同时测定地表水中多种药物及个人护理品

采用快速液相色谱-三重四级杆串联质谱仪(UPLC-MS/MS)测定地表水中31种药物及个人护理品,通过优化分析条件,使方法在0.01μg/L～10.0μg/L范围内线性良好,方法检出限为0.2 ng/L～1.2 ng/L。地表水样品两个质量浓度水平的加标回收率为64.8%～125%,测定6次结果的RSD≤11%。将该方法用于上海市两条河道中10个水样的测定,结果地西泮、氟康唑、甘宝素、咖啡因、可替宁、氨基比林的测定值为6.56 ng/L～302 ng/L,其余PPCPs未检出。     

全自动固相萃取-GC-MS/MS法测定水中多氯联苯

采用全自动固相萃取-气相色谱/三重四极杆串联质谱法(SPE-GC-MS/MS)分析水中7种指示性多氯联苯,通过优化测定条件,使PCBs在0.100μg/L～100μg/L范围内线性良好,方法检出限为0.07 ng/L～0.1 ng/L,回收率为72.1%～102%,RSD为5.8%～12.9%。将该方法用于实际水样测定,结果城市污水处理厂的出水中PCBs检出率较高,而废旧电容器封存点周边地表水易受到PCBs的污染。     

Determination of glyphosate residue in maize and rice using a fast and easy method involving liquid chromatography–mass spectrometry (LC/MS/MS)

A fast and easy method was developed for the determination of glyphosate in maize and rice by using liquid chromatography triple quadrupole mass spectrometry with a Dionex Ion Pack column and phosphate buffer mobile phase. Samples were extracted with an acidified methanol solution. An isotope-labeled internal standard was added to the sample before extraction to ensure accurate tracking and quantification. The method’s performance was evaluated through a series of assessments to determine the accuracy, precision, linearity, matrix effect, limit of detection (LOD), and limit of quantification (LOQ). The mean recoveries for both matrices were within 70–105% at three fortification levels, including the LOQ. The precision for replicates was <20% (RSD%) for both matrices. Good linearity (R²=0.9982) was obtained over the concentration range of 0.01–1.5?mg kg^?1. The LOD was determined to be 0.002?mg kg^?1 for rice and 0.004?mg kg^?1 for maize. The LOQ was 0.01?mg kg^?1 for both maize and rice. Due to its versatility, the proposed method could be considered useful for the determination of glyphosate in cereals in routine analysis.     

SUMMA罐采样-GC/MS法测定吸烟室内空气中挥发性有机物

采用空气预浓缩与气相色谱/质谱联用技术对空气中59种痕量挥发性有机化合物进行定性与定量分析,应用研究的技术对吸烟室烟草空气中的挥发性有机物成分定性解析,对59种常见挥发性有机污染物定量检测.室内环境烟草空气中检出多种挥发性有机污染物,主要有烯烃、烷烃、苯系物等有害成分,不仅对被动吸烟人群造成危害,同时也影响大气环境质量...     

Determination and health risk assessment of enrofloxacin,flumequine and sulfamethoxazole in imported Pangasius catfish products in Thailand

The goals of this study were to determine the levels of three antibiotics – enrofloxacin, flumequine and sulfamethoxazole – in Pangasius catfish products imported into Thailand and to assess the health risks from consumption. To extract these antibiotic residues, acetonitrile, methanol and a small amount of formic acid were used as solvents. Determination of the antibiotics after extraction steps was carried out by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) technique. The results showed that 14 and 3 samples of Pangasius catfish products were contaminated with enrofloxacin and sulfamethoxazole, respectively. No flumequine residue was found. While the concentration levels of these antibiotics in most contaminated samples were lower than the European Union (EU) standard, one sample was found to contain sulfamethoxazole at 245.91 µg kg^?1, which was higher than the EU standard (100 µg kg^?1), indicating the likelihood that some contaminated freshwater fish products are widely distributed in Thai markets. Notably, the concentration levels of enrofloxacin in samples of Pangasius catfish with skin were higher than in non-skin products, suggesting that products with skin might retain more antibiotic residues than non-skin products. Although the hazard quotient showed that consuming imported Pangasius catfish products, based on the current consumption rate, will not adversely affect consumer health, antibiotic residues in Pangasius catfish products imported into Thailand should be continually monitored.