1.5%OV-17+2%QF-1 GB/T 5009.19-1996 食品中六六六、滴滴涕残留量的测定安捷伦7820A玻璃柱

名称：安捷伦7820A玻璃柱

规格：2m*1/4，80-100目

型号：1.5%OV-17+2%QF-1/Chromosorb AW DMCS（80-100目）

编号：20220818001

温度：240°C

应用：GB/T 5009.19-1996 食品中六六六、滴滴涕残留量的测定

本标准规定了食品中六六六、滴滴涕残留量的测定方法。

本标准适用于各类食品中六六六、滴滴涕残留的测定。

1 主题内容与适用范围

  本标准规定了食品中六六六、滴滴涕残留量的测定方法。

  本标准适用于食品中六六六、滴滴涕残留量的测定。

  气相色谱法检测限：?—666、?—666、?—666、?—666依次为0.2，0.8，0.3，0.4?g/kg。

  p，p′-DDE、o，p′-DDT、p，p′-DDD、p，p′-DDT依次为0.5，2.7，1.6，4.0?g/kg。

  薄层色谱法低检测量为0.02?g，适宜范围为0.02～0.20?g。

  篇 气相色谱法(法)

  2 原理

  样品中六六六、滴滴涕经提取、净化后用气相色谱法测定，与标准比较定量。电子捕获检测器对于负电极强的化合物具有较高的灵敏度，利用这一特点，可分别测出微量的六六六和滴滴涕。不同异构体和代谢物可同时分别测定。

  出峰顺序：?-666、?-666、?-666、?-666、p，p′-DDE、o，p′-DDT、p，p′-DDD、p，p′-DDT。

  3 试剂

  使用的试剂一般系分析纯，有机溶剂需经重蒸馏。

  3.1 丙酮。

  3.2 正己烷。

  3.3 石油醚：沸程30～60℃。

  3.4 苯。

  3.5 硫酸。

  3.6 无水硫酸钠。

  3.7 硫酸钠溶液(20g/L)。

  3.8 六六六、滴滴涕标准溶液：准确称取甲、乙、丙、丁六六六四种异构体和p，p′-滴滴涕、p，p′-滴滴滴、p，p′-滴滴伊、o，p′-滴滴涕(?-666、?-666、?-666、?-666、p，p′-DDT、p，p′-DDD、p，p′-DDE、o，p′-DDT)各10.0mg，溶于苯，分别移入100mL容量瓶中，加苯刻度，混匀，每毫升含农药100.0?g，作为储备液存于冰箱中。

  3.9 六六六、滴滴涕标准使用液：将上述标准储备液以己烷稀释适宜浓度，一般为0.01?g/mL。

  4 仪器

  4.1 小型粉碎机。

  4.2 小型绞肉机。

  4.3 组织捣碎机。

  4.4 电动振荡器。

  4.5 旋转浓缩蒸发器。

  4.6 吹氮浓缩器。

  4.7 气相色谱仪，具有电子捕获检测器(ECD)。

GB/T 5009.19-1996 食品中六六六、滴滴涕残留量的测定安捷伦7820A玻璃柱 测试谱图：


GB/T 5009.19-1996 Determination of hexahexahexanol and DDT residues in food Agilent 7820A glass column
GB/T 5009.19-1996 Determination of 6666 and DDT residues in food Agilent 7820A glass column Details:

Name: Agilent 7820A glass column

Specifications: 2m*1/4, 80-100 mesh

Model: 1.5%OV-17+2%QF-1/Chromosorb AW DMCS (80-100 mesh)

No.: 20220818001

Temperature: 240°C

Application: GB/T 5009.19-1996 Determination of 666 and DDT residues in food



This standard specifies the determination methods of hexachloropyridine and DDT residues in food.

This standard applies to the determination of 666 and DDT residues in various foods.




1 Subject content and scope of application

   This standard specifies the determination method of hexachloropyridine and DDT residues in food.

   This standard is applicable to the determination of hexachloropyridine and DDT residues in food.

  The detection limit of gas chromatography: ?-666, ?-666, ?-666, ?-666 are 0.2, 0.8, 0.3, 0.4?g/kg.

  p, p'-DDE, o, p'-DDT, p, p'-DDD, p, p'-DDT were 0.5, 2.7, 1.6, 4.0?g/kg in sequence.

The minimum detection amount of   thick layer chromatography is 0.02μg, and the suitable range is 0.02～0.20μg.

  Part 1 Gas Chromatography (Method 1)

  2 Principle

  The 666 and DDT in the sample were extracted and purified, and then determined by gas chromatography, and quantitatively compared with the standard. Electron capture detectors have high sensitivity to compounds with strong negative electrodes. Using this feature, trace amounts of hexahexahexanol and DDT can be detected respectively. Different isomers and metabolites can be determined simultaneously and separately.

   Peak order: ?-666, ?-666, ?-666, ?-666, p, p'-DDE, o, p'-DDT, p, p'-DDD, p, p'-DDT.

  3 Reagents

   The reagents used are generally of analytical grade, and the organic solvent needs to be redistilled.

  3.1 Acetone.

  3.2 n-hexane.

  3.3 Petroleum ether: boiling range 30～60℃.

  3.4 Benzene.

  3.5 Sulfuric acid.

  3.6 Anhydrous sodium sulfate.

  3.7 Sodium sulfate solution (20g/L).

3.8 Standard solution of DDT and DDT: accurately weigh four isomers of A, B, C, DDT and p,p′-DDT, p,p′-DDT, p,p′-DDT Dyi, o, p'-DDT (?-666, ?-666, ?-666, ?-666, p, p'-DDT, p, p'-DDD, p, p'-DDE, o, p '-DDT) 10.0 mg each, dissolved in benzene, transferred to 100 mL volumetric flasks, added benzene to the mark, mixed well, each milliliter contained 100.0 g of pesticide, and stored in the refrigerator as a stock solution.

  3.9 666. DDT standard solution: Dilute the above standard stock solution with hexane to an appropriate concentration, generally 0.01?g/mL.

  4 Instruments

  4.1 Small grinder.

  4.2 Small meat grinder.

  4.3 Tissue masher.

  4.4 Electric oscillators.

  4.5 Rotary Concentrator Evaporator.

  4.6 Nitrogen blowing concentrator.

  4.7 Gas chromatograph with electron capture detector (ECD).

GB/T 5009.19-1996 Determination of 666 and DDT residues in food Agilent 7820A glass column Test spectrum: