HPLC法测定不同产地赤芍中芍药苷的含量及重金属和残留农药的分析

HPLC Method for Determining the Contents of Paeoniflorin and Analyzing the Heavy Metal and Pesticide Residue in Radix Paeoniae Rubra from Different Areas

目的：建立HPLC法测定不同产地赤芍中芍药苷的含量并对赤芍中重金属和残留农药进行分析.方法：采用反相高效液相色谱法,色谱柱：SunFireTM-C18色谱柱（4.6mm×150mm,5μm）；流动相：甲醇-0.05moL/L磷酸二氢钾（32：68）；检测波长：230nm；柱温：25℃；流速：1.0mL/min；进样量：10μL.采用原子吸收分光光度法测定铅、镉、铜、砷、汞的含量；气相色谱法测定农药残留量.结果：芍药苷的线性范围为0.101 6～1.016mg/mL,r=0.999 8（n=5）；平均加样回收率为101.70％,RSD为2.00％（n=9）,15个产地赤芍中芍药苷含量为1.86％～4.49％.铅、镉、铜、砷、汞残留量分别为0.103～0.548,0.104～0.275,0.474～4.984,0.026～0.352,0.018～0.105mg/kg；BHC、DDT、PCNB残留量分别为11.94×10-3～60.35×10-3、8.19×10-3～154.03×10-3、4.73×10-3～36.62×10-3mg/kg.结论：15个产地赤芍中芍药苷含量均符合2010版《中国药典》；15个产地赤芍药材中均有一定量的重金属及农药残留,重金属含量均符合国家行业标准《药用植物及制剂进出口绿色行业标准》,而其中1个产地DDT残留量超过此标准.

Objective：To establish an HPLC method for the determination of paeoniflorin from Radix Paeoniae Rubra in different habitats and analysis of heavy metals and pesticide residues.Methods：Adopt RP-HPLC,SunFireTM-C18 column（4.6mm×150mm,5 μm）;mobile phase was methanol-0.05mol/L potassium dihydrogen phosphate（32：68）;detection wavelength：230 nm;column temperature：25 ℃;the flowing rate was 1.0mL/min;injection volume：10μL.By atomic absorption spectrophotometric determination of the content of lead,cadmium,copper,arsenic,mercury;gas chromatographic method for the determination of the amount of pesticide residue.Results：The linear range of paeoniflorin was 0.101 6 to 1.016mg/mL,r=0.999 8（n=5）;average recoveries 101.70 ％,RSD 2.00％（n=9）,Radix Paeoniae Rubra paeoniflorin from 15 different areas was from 1.86％ to 4.49％.Lead,cadmium,copper,arsenic and mercury residues were 0.103～0.548,0.104～0.275,0.474～4.984,0.026～0.352,0.018～0.105mg/kg;residues of the BHC,DDT,PCNB were 11.94×10-3～60.35×10-3,8.19×10-3～154.03×10-3,4.73×10-3～36.62×10-3mg/kg.Conclusion：Radix Paeoniae Rubra paeoniflorin from 15 different areas meets the 2010 edition of Chinese Pharmacopoeia;the 15 origin Radix Paeoniae Rubra herbs have certain contents of heavy metals and pesticide residues;heavy metal contents are in line with national industrial standard ＂ Green Trade Standards of Importing ＆ Exporting Medicinal Plants ＆ Preparations ＂,and only in one origin the DDT residues exceed this standard.