GC-ECD 及 GC-MS 法测定祖卡木颗粒及其部分原料药中20种有机氯农药残留量

摘要

Objective To establish a method for determination of 20 organochlorine pesticide residues in Zukamu Granules and part of its crude drug.Methods Acetonitrile and CARBON/PSA SPE were used to extract and purify Zukamu Granules and part of its crude drug,ECD and MS were introduced as the detec-tions respectively,the column DB-5MS was used for the separations of target pesticides,column flow was at 1 mL/min,the inlet was set at 230℃ and ECD at 300℃,ion source was EI,electron energy was at 70eV,and the source temperature was set at 240℃,transfer line and quadrupole were set at 250℃ and 150℃,scan mode was used,the range is m/z 45 ~ 400.Results 20 organochlorine pesticide were separated well by this method (Resolution ≥ 1.512),the recovery rate was at the range of 72.4% ~108.9%,there were good linear relationships between the peak area and concentration at the range of 0.002~0.500 μg/mL (R 2 ≥0.997 1).Conclusion The method is simple,accurate reliable,and can provide ref-erence basis for improving quality standard of Zukamu Granules.%目的：建立测定维药祖卡木颗粒及其部分原料药中20种有机氯农药残留的气相色谱法和气质联用法。方法分别采用乙腈、CARBON／PSA 固相萃取柱对祖卡木颗粒及其部分原料药进行提取和净化，MS 和ECD 分别进行检测，根据色谱保留时间和质荷比信息对样品进行定性分析，GC-ECD 法进行定量分析。以 DB-5MS 色谱柱对待测组分进行分离，柱温采用程序升温方式，柱流量1 mL／min，进样口温度230℃，ECD 温度300℃；离子源为 EI 源，解离电压70 eV，离子源温度240℃，传输线温度250℃，四级杆温度150℃，采用 SCAN 模式，扫描质荷比范围 m／z 45～400。结果20种有机氯农药分离良好（分离度≥1．512），各组分平均回收率为72．4％～108．9％（n ＝6），有机氯类农药在0．002～0．500μg／mL 浓度范围内呈良好的线性关系（r 2≥0．9971）。结论该方法简便、准确且可靠，可以为祖卡木颗粒质量标准的完善提供参考依据。