鸡蛋和“小众”禽蛋中氟虫腈及其代谢物残留状况调查

目的 了解鸡蛋和“小众”禽蛋中氟虫腈及其代谢物的残留状况。方法 采用超高效液相色谱-电喷雾串联质谱法对近年于江西市场上采样的159批市售鲜禽蛋中氟虫腈及其3种代谢物进行了检测,分析了不同蛋种中氟虫腈及其代谢物的残留状况。结果 159批样本中共检出35批仅含有4种化合物中的一种,且仅检出氟甲腈和氟虫腈砜两种代谢物,氟虫腈砜主要是鸡蛋和鹌鹑蛋检出,检出率12.6%,氟甲腈主要是鸭蛋检出,检出率9.4%。结论 鲜禽蛋中氟虫腈及其代谢物的残留量远低于国内外限量,安全尚可,但整体检出的样本数依然提示出要密切关注家禽养殖圈杀虫剂的使用。     

固相萃取-气质联用法测定蔬菜中氟虫腈和溴虫腈残留

目的建立蔬菜中氟虫腈和溴虫腈残留的固相萃取-气相色谱/质谱分析方法。方法试样经乙腈提取,硫酸镁和氯化钠盐析,通过比较PSA柱、石墨化碳/NH_2柱、中性氧化铝柱、Qu Ch ERS净化管4种小柱,对蔬菜中氟虫腈和溴虫腈的吸附和净化情况,选取PSA固相萃取柱进行净化,GC-MS测定,外标法定量。结果该方法在5μg/L~100μg/L具有良好的线性关系(相关系数均0.999),氟虫腈和溴虫腈的回收率分别为93.1%~99.2%和97.4%~100.0%,相对标准偏差(RSD)分别为3.5%~8.6%、2.8%~6.1%,检出限为1.0μg/kg~2.0μg/kg,定量限为3.0μg/kg~6.0μg/kg。应用该方法对90份蔬菜样品进行分析,检出2份阳性样品。结论该方法的灵敏度、精密度和LOD均符合残留分析要求,具有简便、准确、成本低的特点,适用于蔬菜中氟虫腈和溴虫腈农药残留的检测。     

凝胶净化色谱-三重四级杆串联气相色谱质谱法检测植物源性食品中氟虫腈及其代谢物残留量

目的采用凝胶净化色谱-三重四级杆串联气相色谱质谱法(GPC-GC/MS/MS)对植物源性食品中氟虫腈及其代谢物氟甲腈、氟虫腈亚砜、氟虫腈砜农药残留量进行分析。方法样品经乙腈超声提取后采用QuECHRS萃取包净化,用SH-Rxi-5il MS(30 m×0.25 mm,0.25μm)毛细管色谱柱分离,外标法定量分析。结果用本法测定,氟虫腈及其代谢物氟甲腈、氟虫腈亚砜、氟虫腈砜色谱峰得到很好的分离,在0.01μg/ml^0.5μg/ml浓度内呈现良好的线性关系。相关系数均达到0.9999,方法检出限均为0.003 mg/kg,氟虫腈及其代谢物在3个浓度添加水平下的加标回收率为89%~116%,相对标准偏差在1.10%~7.22%。结论该方法实现了氟虫腈及其代谢物检测的自动化、快速、高灵敏度和高稳定性分析,能够满足目前植物源性食品中氟虫腈及其代谢物残留检测限量的要求。     

土壤中6种白蚁防治药物的超高效液相色谱检测方法研究

目的建立超高效液相色谱法(UPLC)测定土壤中6种白蚁防治药物——吡虫啉、氟虫腈、虫螨腈、毒死蜱、氰戊菊酯、联苯菊酯残留量的分析方法。方法样品用乙腈匀浆提取,经离心、NH2固相萃取小柱净化、浓缩、定容后,采用超高效液相色谱法进行测定,外标法定量。结果所有农药在0.01~5.00 mg/L范围内线性关系均良好,相关系数r20.99;所有农药的方法检出限均低于10μg/kg;在0.050 0、0.167和0.500 mg/kg添加水平下,样品平均回收率为83.0%~117.0%,相对标准偏差RSD为2.0%~4.4%。结论本方法简便,重现性良好,可用于土壤中吡虫啉、氟虫腈、虫螨腈、毒死蜱、氰戊菊酯、联苯菊酯6种药剂残留的检测。     

高效液相色谱-串联质谱法测定蔬菜中氟虫腈及其代谢物残留

目的 建立了蔬菜中氟虫腈及其代谢物氟甲腈、氟虫腈砜和氟虫腈亚砜的高效液相色谱-串联质谱法。方法 用乙腈超声提取样品中的氟虫腈及其代谢物,高速离心后,提取液经QuChERS净化管净化,过0.22μm滤膜,经Waters Acquity UPLC HSS T3色谱柱分离,以乙腈-0.1%甲酸水(含5mmol/L乙酸铵)做流动相,梯度洗脱,采用电喷雾离子源负离子检测模式(ESI-)和多重反应监测(MRM)模式测定,基质匹配标准曲线定量。结果 在蔬菜基质中,被测物在1.0 μg/L～100 μg/L内相关系数均>0.999,平均回收率范围为97.8%～109%,相对标准偏差(RSD)为1.0%～7.7%,检出限为0.02μg/kg～0.10μg/kg,定量限为0.06μg/kg～0.30μg/kg。结论 该方法操作简单、准确、快速、灵敏度高,适用于蔬菜中氟虫腈及其代谢物残留的检测。     

液相色谱-串联质谱检测鸡蛋中氟虫腈及其代谢物的残留量

目的建立一种检测鸡蛋中氟虫腈及其代谢物残留的液相色谱-串联质谱(LC-MS/MS)定量分析方法。方法优化检测条件:用乙腈进行样品提取,选择C18固相萃取小柱和无水硫酸镁对提取样品净化后进行液质联用检测。结果经过优化后液相条件:流动相由2mmol/L的甲酸铵水溶液和甲醇组成,采用梯度洗脱方式在C18反相色谱柱中进行分离,进样量为4μL。质谱条件:离子源采用ESI负离子,通过SRM模式对样品中氟虫腈及其代谢物进行定量检测。优化后,氟虫腈及其代谢物在0~20ng/mL质量浓度范围内线性关系良好,R2均>0.9993,检出限(S/N=3)和定量限(S/N=10)分别0.2~0.4μg/kg和0.66~1.32μg/kg。实际样品中添加4.0、20.0、40.0μg/kg 3个质量浓度水平下,平均回收率在76.60%~98.24%,相对标准偏差(RSD)为1.03%~3.41%,符合定量检测要求。结论该方法操作简便、灵敏度高,可满足鸡蛋中氟虫腈及其代谢物的检测要求。     

Sin-QuEChERS结合液相色谱串联质谱法测定白蚁预防工程土壤中吡虫啉和氟虫腈残留

目的 建立一种测定白蚁预防工程土壤中吡虫啉和氟虫腈残留的Sin-QuEChERS结合液相色谱串联质谱分析方法。方法 预防工程土壤经0.1%甲酸-乙腈提取后,经Sin-QuEChERS Nano净化柱净化,流动相由2 mmol/L乙酸铵水溶液(含0.1%甲酸)、甲醇进行梯度洗脱,采用串联质谱(MS/MS)多反应监测模式(MRM)对样品进行检测,采用外标法进行定量分析。结果 吡虫啉、氟虫腈在0.002～0.5 mg/L范围内线性关系良好,吡虫啉相关系数(R²)为0.998 0,氟虫腈(R²)为0.998 6。以新建预防工程土壤为基质,在0.02、0.05、0.2 mg/kg水平下,吡虫啉和氟虫腈的添加回收率范围在80.5%～93.5%之间,相对标准偏差(RSD)在4.62%～9.17%之间(n=6),两种药物的定量限(LOQ)均为0.003 mg/kg,检出限(LOD)均为0.001 mg/kg。结论 本方法操作简单,重现性好,适用于新建房屋白蚁预防工程土壤中吡虫啉和氟虫腈的同时快速测定与定量分析。     

河虾体中氟虫腈残留量气相色谱法测定

氟虫腈(Fipronil)是法国罗纳普朗克公司开发的苯基吡唑类新型高效广谱性杀虫剂，对于稻田害虫防治效果较好。但对哺乳动物有神经毒性，在环境中难于分解，在土壤中半衰期达1～3个月，在水中为134d。由于对土壤和水体的污染，氟虫腈在河虾养殖过程中的残留量可能对人体产生危害。本文对河虾氟虫腈残留量的测定方法进行了改进。     

应用QuEChERS技术与气相色谱-串联质谱法同时检测南果梨中16种农药残留

目的建立南果梨中霜霉威、氧乐果、特丁硫磷、西玛津、抗蚜威、噻节因、氟虫腈、二甲戊灵、氟菌唑、嘧菌环胺、虫螨腈、吡草醚、噁霜灵、溴螨酯、三氯杀螨砜及精噁唑禾草灵等16种农药残留同时检测的QuEChERS-气相色谱-串联质谱分析方法。方法使用乙腈提取样品中的农药,经N-丙基乙二胺(PSA)分散固相萃取净化,再经气相色谱-三重四级杆串联质谱分析。结果 16种农药在线性范围内相关系数均大于0.994。方法检出限范围(S/N=3)为0.01～1.62μg/kg,方法定量限范围为0.02～5.40μg/kg。当加标水平为62.5μg/kg时,其回收率在78.5%～98.6%之间,相对标准偏差(RSD)在3.8%～11.4%之间。结论该方法具有操作简单、快速、灵敏的特点,适用于南果梨中农药多残留的检测。     

联苯菊酯、溴虫腈和氟虫腈三种农药残留质控样品的制备与评价——以卷心菜粉为例

【目的】研究制备适合于蔬菜基质中农药残留检测的能力验证样品,通过能力验证评价相关实验室检测能力。【方法】选择卷心菜为样品基质,采用冷冻干燥、标准添加的方式制备能力验证样品,通过随机抽样测定以评估样品的均匀性,通过观察样品42天内目标化合物测试结果变化以评估样品的稳定性。【结果】样品均匀性及稳定性检验符合预期效果,制备的能力验证样品定值准确。【结论】制备的联苯菊酯、溴虫腈和氟虫腈能力验证样品,可用于蔬菜中农药残留的能力验证和方法评价,结果满意。     

Fate of Fipronil and its Metabolites in/on Grape Leaves, Berries and Soil Under Semi Arid Tropical Climatic Conditions

Fate of fipronil and its major metabolites fipronil sulfide (MB 45950), fipronil-desulfinyl (MB 46513) and fipronil sulfone (MB 46136) were studied in/on grape leaves, berries and soil. As initial residue deposits on the leaves the major component was that of fipronil, while all the 3 metabolites were also present. Among metabolites residues of MB 46513 was highest followed by MB 46136 and MB 45950. In leaves fipronil degraded faster than its metabolites. The residues of fipronil in leaves degraded at the half-life of 9.6 and 18.3 days and that of total fipronil (sum of fipronil and its metabolites) at 13.6 and 20 days, from treatment at recommended and double the recommended dose, respectively. At the time of harvest in leaves, grape berries and soil residues of fipronil and all its metabolites were below the quantifiable limit of 0.01 mg kg^?1.     

高效液相色谱法测定黄瓜中嘧霉胺和烯酰吗啉农药残留

[目的]研究黄瓜中嘧霉胺和烯酰吗啉残留量的检测方法。[方法]采用乙腈提取黄瓜中的嘧霉胺和烯酰吗啉农药残留,氟罗里硅土固相萃取小柱进行柱净化,高效液相色谱可变波长紫外检测器（260nm）进行测定。[结果]嘧霉胺和烯酰吗啉回收率分别为97．74％～102．83％和83．21％,103．74％,相对标准偏差均〈5％,最低检出限分别为0．008mg／kg和0．014mg／kg。[结论]该方法简单、快捷、灵敏,适合于黄瓜中嘧霉胺和烯酰吗啉残留量的测定。     

Persistence and Metabolism of Fipronil in Rice (Oryza sativa Linnaeus) Field

Rice is one of the most important food crops worldwide. However, it is also a valuable tool in assessing toxicity of organic and inorganic compounds. Fipronil insecticide has been widely used to control rice pests. The research was conducted to evaluate the fate of fipronil in rice-field. Persistence and metabolism of fipronil in rice is studied by applications of Regent 0.3G @ 45 and 180 g a.i. ha^?1 was made 7 days after transplanting of paddy. Samples of paddy plants were collected at 7, 15, 30, 45, 60, 90 and 120 days after the application of insecticide. The samples of rice grains, bran, husk and straw were collected at the time of harvest. The samples were extracted and cleaned up by following a standardized methodology. Fipronil and its metabolites were quantified by gas liquid chromatography and confirmed by gas chromatography mass spectrometer. The total residues of fipronil and its metabolites in paddy plants after 7 days of its application at recommend and four times of recommend doses were found to be 6.60 and 19.85 mg kg^?1, respectively. Among fipronil metabolites, sulfone derivative had maximum residue concentration followed by other metabolites viz. sulfide, amide and desulfinyl. The residues were reached below the detectable limit (0.01 mg kg^?1) after 45 and 90 days at recommend and four time of recommend doses, respectively. At harvest, the samples of paddy straw, rice grains, bran and husk did not reveal the presence of fipronil and its metabolites.     

PXC和EMR-Lipid QuEChERs技术在动物源性食品中多种β-受体激动剂残留检测的前处理效果对比

目的 比较PXC和EMR-Lipid QuEChERs(简称EMR-L)萃取法对动物源性食品中多种β-受体激动剂残留检测效果的影响.方法 利用UPLC-MS/MS分析技术,使用PXC固相萃取小柱和EMR-Lipid QuEChER两种前处理材料,对相同样品的检测结果进行对比和分析.结果 两种前处理方法在0.5～10 n...     

Operational note effects of fipronil and lambda-cyhalothrin against larval Anopheles quadrimaculatus and nontarget aquatic mosquito predators in Arkansas small rice plots

The effects of fipronil and lambda-cyhalothrin, applied at rates labeled for control of the rice water weevil, Lissorhoptrus oryzophilus, on 3 nontarget indigenous insect species in Arkansas rice are described. Three replicates of untreated control checks and fipronil- and lambda-cyhalothrin-treated plots containing 3 sentinel cages each were performed. Ten 4th-stage larvae of Anopheles quadrimaculatus, 10 adult Tropisternus lateralis, or 10 adult Notonecta indica were placed within individual cages in small rice plots treated with ICON 6.2 FS (fipronil) at 0.025 lb active ingredient (AI)/acre (0.028 kg/ha) or KARATEZ 2.08 CS (lambda-cyhalothrin) at 0.03 lb AI/acre (0.033 kg/ha) applied over vegetation and water with a single-boom sprayer. At 24 h after treatment in fipronil plots, significantly higher control of An. quadrimaculatus and T. lateralis (69 and 48% control, respectively) was achieved, compared to N. indica (18%). In lambda-cyhalothrin plots 24 h after treatment, 100% reductions of both T. lateralis and N. indica were highly significant (P < 0.05) from the lower level of control in An. quadrimaculatus (10%). At 48 h after treatment, no significant, differences existed between all species within fipronil plots, with An. quadrimaculatus, T. lateralis, and N. indica obtaining 41, 10, and 7% control, respectively. Significantly higher (P < 0.05) control was obtained in lambda-cyhalothrin plots 48 h after treatment, with 93 and 53% control of T. lateralis and N. indica, respectively, compared to 7% control of An. quadrimaculatus. A marked difference in susceptibility was found between selected nontarget organisms used in this study. When using lambda-cyhalothrin to control adult L. oryzophilus, populations of nontarget beneficial insects, such as T. lateralis and N. indica, could be adversely affected, whereas nontarget pestilent species, such as An. quadrimaculatus, could proliferate. Fipronil achieved higher percentages of control against An. quadrimaculatus, compared to lambda-cyhalothrin, and was less harmful to both nontarget predators.     

4种杀虫剂毒饵对黑翅土白蚁的防治效果

目的了解4种杀虫剂配制的毒饵对黑翅土白蚁的防治效果,为控制黑翅土白蚁的危害提供新的手段。方法将阿维菌素、氟虫腈、灭蚁灵和吡虫啉4种药剂分别配制成1%和0.2%的毒饵,每袋毒饵包3g,采用正交试验筛选出的最佳毒饵应用技术,进行林间诱杀药效试验。结果用药后4周1%氟虫腈与0.2%阿维菌素毒饵的防治效果分别为99.33%和91.32%,显著高于其他各处理组。用药4周后,在1%氟虫腈和0.2%阿维菌素毒饵试验区出现白蚁巢穴死亡指示物——鹿角菌,进一步证实了1%氟虫腈和0.2%阿维菌素毒饵的防治效果。结论 1%氟虫腈毒饵和0.2%阿维菌素毒饵可用于林地黑翅土白蚁的防治。