出口柑桔中双甲脒及代谢物残留量测定

柑桔样品中双甲脒及代射物在酸性条件下回流水解成2，4－二甲基苯胺，正己烷提取，酸，碱反复液－液分配净化，七氟丁酸酐将2，4－二甲基苯胺衍生成2，4－二甲苯七氟丁酰胺，用配有电子俘获检测器的气相色谱仪测定，外标法定量。     

纸品中多氯联苯的气相色谱法测定

建立了一种纸品中多氯联苯的气相色谱分析方法,该方法利用碱溶液对纸中的干扰物进行破坏,用C18固相萃取柱和浓硫酸进行净化,采用GC-ECD对萃取液进行分析。该方法线性范围广,检测限低,加标回收率为95.30%～100.10%,精密度实验RSD为1.79%～3.30%,完全可以满足纸品中多氯联苯检测的需要。     

正交法测定菠萝罐头中二溴乙烷残留量

建立了菠萝罐头中二溴乙烷残留量的正交测定方法。样品前处理采用正交法优化正己烷-丙酮混合提取液配比及盐添加量。通过比较回收率表明:影响提取效果的主次顺序为蒸馏溶剂及体积配比>无水硫酸钠添加量>蒸馏水添加量。实验结果确定的最佳蒸馏提取条件为:无水硫酸钠添加量20g,蒸馏水添加量100mL,蒸馏溶剂及体积配比正己烷-丙酮(2:1)。在2、5、10、20μg/kg4个水平添加回收实验中,平均回收率(n=5)为91.52%～106.33%;相对标准偏差均小于10%,方法检出限(MDL)为0.5μg/kg。实验表明:该方法简便、快速、灵敏、准确,适用于菠萝水果罐头样品的二溴乙烷农药残留分析。     

Validation of a headspace solid-phase microextraction procedure with gas chromatography-electron capture detection of pesticide residues in fruits and vegetables

Headspace solid-phase microextraction (HS-SPME) was evaluated for the determination of pesticide residues in fruits and vegetables by gas chromatography with an electron capture detector (GC-ECD). The fibre used was coated with polydimethylsiloxane (100 μm thickness) and the analytical conditions employed have been developed and optimised in a previous work [Chai, M. K., Tan, G. H., & Asha, L. (2008). Optimisation of headspace solid-phase microextraction for the determination of pesticide residues in vegetables and fruits. Analytical Sciences, 24 (2), 273–276]. The results show that the HS-SPME procedure gave a better linear range, accuracy, precision, detection and quantification limits and is adequate for analysing pesticide residues in fruits and vegetables. The average recoveries obtained for each pesticide ranged between 71% and 98% at three fortification levels with the relative standard deviation of less than 5%. Repeatability (0.3–3.7%) and intermediate precision (0.8–2.5%) were shown to be satisfactory. The limits of detection (0.01–1 μg L⁻¹) and the limits of quantification (0.05–5 μg L⁻¹) of these pesticides were much lower than the maximum residue levels (MRL), allowed for fruits and vegetables in Malaysia.     

Concentrations and determinants of organochlorine levels among pregnant women in Eastern Spain

Persistent organic pollutants (POPs) comprise a large variety of toxic substances with ample distribution. While exposure to these toxins occurs mainly through diet, maternal POP levels may be influenced by certain sociodemographic, environmental, or lifestyle factors. This is important given that these substances may have adverse effects on fetal development. The aim of this study is to examine the sociodemographic, environmental, lifestyle, and dietary determinants of the levels of hexachlorobenzene (HCB), b-hexachlorocyclohexane (b-HCH), 1,1,1-trichloro-2,2-bis(4-chlorophenyl)ethane (4,4′-DDT), 1,1-dichloro-2,2-bis(4-chlorophenyl)ethylene (4,4′-DDE), and polychlorinated biphenyls (PCB congeners 118, 138, 153, 180) measured in the blood of pregnant women participating in a mother-child cohort study conducted in Valencia (Spain).The study population consisted of 541 pregnant women who formed part of the INMA (Childhood and the Environment) cohort (2004-2006). POP levels were determined in blood taken during the 12th week of pregnancy with the aid of gas chromatography with electron capture detection. Sociodemographic, environmental, and dietary information was obtained from a questionnaire. Multivariate Tobit regression models were constructed in order to assess the association between POP levels and selected covariates.The results showed that all the women had detectable levels of at least one of these compounds while in 43% of the subjects, all eight compounds were detected. The compounds found in the greatest number of women were 4,4′-DDE (100%) and PCBs 153 and 180 (95%). The most important determinants of high POP levels were the mother's age, country of origin, increased body mass index, and number of weeks of breastfeeding after previous pregnancies. With regard to diet, 4,4′-DDT and 4,4′-DDE levels increased with the intake of meat, fruit, and cereal. PCB 153 levels increased with the intake of seafood. The levels of HCB, b-HCH, 4,4′-DDT, and 4,4′-DDE observed in this study were slightly higher than in other studies, whereas the PCB levels were similar.     

Quantitative GC-ECD Analysis of Halogenated Metabolites: Determination of Surface and Within-Thallus Elatol of Laurencia obtusa

Information on natural concentrations or variability of secondary metabolites in marine organisms may be important both to ecological/evolutionary and applied approaches. A gas chromatographic procedure with an electron capture detector (GC-ECD) was developed to quantify the sesquiterpenoid elatol at the surface and within-thalli of 70 specimens of the red seaweed Laurencia obtusa. The concentration of elatol was highest within-thalli [9.89 mg g⁻¹ of L. obtusa, dry weight (d.w.)], compared to lower values found at the surface [0.006 mg g⁻¹ of L.obtusa (d.w.), or 0.5–10.0 ng cm⁻²]. This method provides a rapid and inexpensive quantification of small quantities of elatol, and probably may also be used to quantify other halogenated compounds usually found in red seaweeds.     

微波辅助萃取-气相色谱法测定茶叶中多种有机氯和拟除虫菊酯农药残留

建立了茶叶中18种有机氯和9种拟除虫菊酯农药残留微波辅助萃取．气相色谱分析方法。运用正交设计法对微波萃取条件进行了优化,茶叶样品用正己烷-二氯甲烷混合溶N（1：2,V／V）进行萃取,萃取液用弗罗里硅土和中性氧化铝混合层析柱净化,采用J＆WDB-1701毛细管柱分离,GC．ECD法同时测定。在0．4、0．2、0．1ml（0．5μg／m1有机氯农药＋1．0μg／ml拟除虫菊酯农药）三个水平添加时的平均回收率（n=5）分别为80．9％～118．5％、88．4％～120．7％、80．9％～116．3％;相对标准偏差分别为2．09％～6．70％、1．89％～6．49％、1．98％～11．87％。该方法的检出限为：有机氯农药0．0004～0．0048mg／kg,拟除虫菊酯农药0．0033～0．0400mg／kg。     

Potential dermal exposure to deltamethrin and risk assessment for manual sprayers: influence of crop type

A comparison of the Potential Dermal Exposure (PDE) of workers to the insecticide deltamethrin was made as a function of crop type, in small agricultural production units in Argentina. Seven experiments were done with two different crops (maize and broccoli, treated area between 600 and 1000 m(2)) with three different operators under typical field conditions using a lever operated knapsack. The methodology is based on the whole body dosimetry technique, presenting separately the data for mixing/loading and application activities. These results indicate a higher concentration of pesticide in lower body sections for broccoli and a wider distribution for maize. The risk inherent in these agricultural procedures is estimated through Margin of Safety (MOS) values and was found to be generally safe. Preliminary results of a mass balance distribution of the pesticide between crop, soil and operator are also presented.     

固相萃取－气相色谱法同时检测茶叶中多种农药和多氯联苯残留

建立茶叶中21种有机氯、拟除虫菊酯类农药和多氯联苯(polychlorinated biphenyls,PCBs)残留固相萃取(solid-phase extraction,SPE)-气相色谱分析方法。用正己烷-丙酮(1:1,V/V)提取,经Envi-Carb/NH2复合固相萃取柱净化,采用RTX-5毛细管柱分离,气相色谱-电子捕获检测器(gas chromatography-electron caputure detector,GC-ECD)检测。在0.02、0.05、0.3mg/kg三个添加水平,平均回收率为68.64%～125.62%,相对标准偏差(relative standard deviation,RSD)为1.05%～12.78%,该方法的检测限(detection of limit,LOD)在0.0022～0.0129mg/kg之间,适用于茶叶试样中痕量残留的分析。     

索氏提取-气相色谱法测定食品纸包装材料中的多氯联苯

建立一种测定食品纸包装材料中多氯联苯的测定方法。采用索氏提取法提取样品,通过浓硫酸净化、无水硫酸钠脱水、浓缩后,用气相色谱-ECD进行测定。并对索氏提取的不同条件进行系统比较,优化实验条件。方法的检出限为0.5 μg/kg,回收率为78%～86%,相对标准偏差小于7%。