潞党参中重金属和农药残留分析

Analysis of Heavy Metals and Pesticide Residues in Codonopsis Radix

目的：建立测定潞党参中重金属的含量和部分农药残留量的方法,并评价太原市售潞党参药材的安全性。方法：采用气相色谱法测定潞党参中9种有机氯农药残留量。色谱柱为DB-1701弹性石英毛细管柱,检测器为63Ni-ECD电子捕获检测器,载气为高纯氮,进样口温度为210℃,检测器温度为300℃,进样量为1μl。采用电感耦合等离子体质谱法测定其中铅、镉、汞、砷含量。高频发射功率为1 500 W,预混室温度为2℃,冷却气流速为15.0 L/min,载气流速为0.8 L/min,蠕动泵速为0.1 ml/s,补偿气流速为0.3 L/min,进样深度为8 mm。结果：9种有机氯农药检测质量浓度线性范围为4～100μg/L（r≥0.995 0）;精密度、稳定性、重复性试验的RSD≤13.7%;加样回收率为97.0%～104.0%（RSD≤1.9%,n=9）。铅、镉、汞、砷检测质量浓度线性范围分别为0～0.025、0～0.025、0～0.005、0～0.025μg/ml（r≥0.999 2）;精密度、稳定性、重复性试验的RSD≤9.3%;加样回收率分别为95.0%～106.7%（RSD≤3.8%,n=9）。结论：该方法简便、灵敏、准确,可用于潞党参中重金属的含量和部分农药残留量的测定。太原市售潞党参药材中重金属含量、有机氯农药残留量均符合国家限量标准。

OBJECTIVE： To establish a method for the determination of heavy metals and pesticide residues in Codonopsis Ra- dix to evaluate the safety of Codonopsis Radix commercially available in Taiyuan city. METHODS： Gas chromatography was used to determine the residues of organochlorine pesticides in Codonopsis Radix. The column was DB-1701 fused silica capillary col- umn, detector was 63Ni-ECD electron capture detector, carrier gas was high-purity nitrogen, volume temperature was 210℃, detec- tor temperature was 300 ℃ and volume injection was 1 μl. ICP-MS method was conducted to determine the contents of Pb, Cd, Hg and As. High frequency transmitter power was 1 500 W, temperature of premix chamber was 2 ℃, flow rate of cooling gas was 15.0 L/min, flow rate of carrier was 0.8 L/min, peristaltic pump speed was 0.1 ml/s, compensation flow rate was 0.3 L/min and volume depth was 8 mm. RESULTS： The linear range of organochlorine pesticides was 4-100 μg/L （r≥0.995 0）. RSDs of pre- cision, stability and reproducibility tests were not higher than 13.7 %, recovery was 97.0 %-104.0 % （RSD≤ 1.9 %, n = 9 ）. Linear re- gression equations of Pb, Cd, Hg and As were 0～0.025,0～0.025,0～0.005,0～0.025 μg/ml（r≥0.999 2）, respectively. RSDs of precision, stability and reproducibility tests were not higher than 9.3%, average recoveries was 95.0%-106.7% （RSD≤3.8%, n= 9）. CONCLUSIONS： The method is simple, sensitive and accurate, and can be used for the determination of heavy metals and parts of pesticide residues in Codonopsis Radix. The contents of heavy metals and organochlorine pesticide residues in Codonopsis Radix are comformed to national limits.