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毛细管柱气相色谱法测定精制马拉硫磷溶液含量
田恺,张浩然,张亦菲,徐汀,华贤辉,商军
0
(上海市兽药饲料检测所)
摘要:
本实验建立了毛细管柱气相色谱法测定精制马拉硫磷溶液含量。采用5%苯基-95%甲基聚硅氧烷为固定相的毛细管柱,柱温230℃,进样口温度250℃,检测器温度265℃,载气:氮气;流速:2 ml/min;进样量1 μL(分流比50:1),内标物质为邻苯二甲酸二丙酯。在上述实验条件下,马拉硫磷峰与内标物质峰分离好(分离度>10);马拉硫磷浓度在35.2~52.8 mg/ml范围内呈良好线性关系,r = 0.9991;方法平均回收率为98.37~100.08%,RSD为0.2~0.3%(n=6);校正因子RSD为0.5%(n=6);供试品溶液在10 h内稳定。本法操作简便、快速、结果准确,应用于实际样品检测,结果满意,可作为精制马拉硫磷溶液含量测定的质控方法。
关键词:  毛细管柱气相色谱法  精制马拉硫磷溶液  含量测定
DOI:
投稿时间:2020-03-21修订日期:2020-07-27
基金项目:
Determination of Malathion in Purified Malathion Solution by Capillary Column Gas Chromatography
(Shanghai Institute for Veterinary Drug and Feeds Control,Shanghai,201103;China)
Abstract:
A method for determination of malathion in purified malathion solution by capillary column gas chromatography was developed. The capillary column with 5% phenyl-95% methylpolysiloxane as stationary phase was used. The column temperature was 230 ℃, the inlet temperature was 250 ℃, the detector temperature was 265 ℃, the carrier gas was nitrogen, the flow rate was 2 ml / min, the injection volume was 1 μL (split ratio 50:1), and the internal standard material was dipropyl phthalate. Under above experimental conditions, malathion peak was well separated from the internal standard substance peak(resolution >10), the calibration curve for malathion was linear in the range of 35.2 ~ 52.8 mg/ml (r = 0.9991), the average recovery of the method was 98.37 ~ 100.08%, and the RSD was 0.2 ~ 0.3%(n = 6), the correction factor RSD was 0.5% (n = 6), the test solution was stable within 10 hours. The results obtained by experimental verification showed that the method is simple, rapid and reliable for determination of malathion in purified malathion solution by capillary column gas chromatography.
Key words:  capillary column gas chromatographic  purified malathion solution  determination of content

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