气相色谱法测定铁皮石斛类保健食品中10种有机磷农药残留  

Determination of 10 kinds of organic ophosphorpus pesticide in dendrobium health food by gas chromatography

作　　者：郑秋岚[1] 贾建萍[1] 张舟艺[1] 李跃中[1] 孙丽华[1] 

机构地区：[1]浙江省医学科学院,浙江杭州310013

出　　处：《中国卫生检验杂志》2015年第18期3067-3069,共3页Chinese Journal of Health Laboratory Technology

基　　金：浙江省科技厅院所专项项目(2015F10014);浙江省营养学医学支撑学科建设(11-ZC03);营养与人体健康关系研究创新团队(续建)(2011F20038)

摘　　要：目的建立气相色谱测定铁皮石斛类保健食品中10种有机磷农药残留的分析方法,为保健食品质量控制提供依据。方法样品经乙腈振荡,匀浆提取后,无水硫酸镁和氯化钠盐析,PSA、C18和无水硫酸镁净化与除水,离心后取上清液,加入分析保护剂(10 mg/mlγ-古洛糖酸内酯溶液),采用DB-1701石英毛细管柱(30 m×0.25 mm,0.25μm)分离,火焰光度检测器(FPD)测定。根据保留时间定性,外标峰面积法定量。结果 10种有机磷农药分离良好,峰面积与浓度呈良好的线性相关性(r>0.999),线性范围为0.02μg/ml^0.10μg/ml,检出限为0.02 mg/kg^0.03 mg/kg,加标回收率为89.3%~111.0%,相对标准偏差(RSD)为4.7%~7.1%。结论本方法检测有机磷农药残留具有操作简单、快捷、结果准确性高的特点,具有较高的实用性,适用于铁皮石斛类保健食品中10种有机磷农药的同时检测。Objective To establish a method for determination of 10 kinds of organic ophosphorpus pesticide in dendrobium health food by gas chromatography, so as to provide basis for the quality control of health food. Methods The sample was sep- arated by quartz capillary column DB - 1701 （30 m × 0.25 mm, 0.25μm） by determined by flame photometric detector （FPD） after acetonitrile shock extraction, salting - out by magnesium sulfate anhydrous and NaC1, purtried and dried by PSA, Cls and magnesium sulfate anhydrous and the supernatant was added to the analysis protection（ 10 mg/ml γ - gulonicacidgamma - lactone solution）. Observational measurement was grounded with retention time, quantity was grounded with external standard method. Results 10 kinds of organic phosphorus pesticides were separated, the peak area and the concentration showed good linearity （r 〉 0. 999）, the linear range of the method was among 0.02 μg/ml- 0.10 μg/ml, the detection limits ranged from 0.02 mg/kg - 0.03 mg/kg, the RSD was among 4.7% - 7.1% with the recovery rates of 89.3 % - 111.0%. Conclusion The method has been proven to he simple, quick, and the results are with high accuracy and practicability, is also suitable for detec- tion of organic ophosphorpus pesticide in dendrobium health food.

关 键 词：气相色谱法 有机磷农药 铁皮石斛 保健食品 

分 类 号：O657.71[理学—分析化学]