无硫党参饮片质量标准的制定与提高
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摘要
目的研究无硫党参饮片的安全性、有效性质量标准,为其质量监控和临床应用提供参考。方法分别采用薄层色谱法、气相色谱法测定来自5个产区的21批无硫党参饮片的水分、总灰分、二氧化硫残留量、浸出物,分别采用原子吸收分光光度法和气相色谱法测定其重金属及有害元素、农药残留量,并采用HPLC建立党参中党参炔苷的含量测定方法。结果 21批党参饮片的二氧化硫残留不超过7mg/kg,铅含量不超过1.124 mg/kg,砷含量不超过0.067 mg/kg,镉含量不超过0.058 mg/kg,汞含量不超过0.003 mg/kg,铜含量不超过14.121 mg/kg,总六六六含量不超过0.03 mg/kg,总滴滴涕含量不超过0.031 mg/kg,五氯硝基苯含量不超过0.008 mg/kg。党参炔苷含量测定平均加样回收率为97.71%,RSD=1.32%,平均质量分数为0.138%。结论无硫党参饮片的安全性指标限量为二氧化硫残留不超过10mg/kg,重金属和农药残留标准符合药典对党参饮片的限量标准,有效性指标含量测定方法可靠,可为党参的质量监控及临床使用提供依据。
Objective To study the safety and effectiveness of quality standards of sulfur-free Codonopsis Radix Decoction Pieces; To provide references for the quality monitoring and clinical application of sulfur-free Codonopsis Radix Decoction Pieces. Methods The check items(water, total ash, sulphur dioxide, and ethanol-soluble extractives) of 21 batches of sulfur-free Codonopsis Radix Decoction Pieces from five producing areas were determined by TLC and GC. Heavy metals, harmful elements and pesticide residues were detected by atomic absorption spectrophotometry and GC. The method for content determination of Lobetyolin in Codonopsis Radix was established by HPLC. Results Safety index check items of 21 batches of Codonopsis Radix Decoction Pieces showed: Sulfur dioxide residue ≤ 7 mg/kg, Pb content ≤ 1.124 mg/kg, As content ≤ 0.067 mg/kg, Cd content ≤ 0.058 mg/kg, Hg content ≤ 0.003 mg/kg, Cu content ≤ 14.121 mg/kg. total BHC ≤ 0.03 mg/kg, total DDT ≤ 0.031 mg/kg, and pentachloronitrobenzene(PCNB) ≤ 0.008 mg/kg. The average sample recovery rate of Lobetyolin content was 97.71%, RSD was 1.32%, and the average fraction was 0.138%. Conclusion The safety index of sulfur-free Codonopsis Radix Decoction Pieces is sulfur dioxide residue ≤ 10 mg/kg. The heavy metal and pesticide residue standards meet the limit standard for Codonopsis Radix in pharmacopoeia. The method for determining the effectiveness index is reliable, which can provide a basis for the quality control and clinical use of Codonopsis Radix.
Objective To study the safety and effectiveness of quality standards of sulfur-free Codonopsis Radix Decoction Pieces; To provide references for the quality monitoring and clinical application of sulfur-free Codonopsis Radix Decoction Pieces. Methods The check items(water, total ash, sulphur dioxide, and ethanol-soluble extractives) of 21 batches of sulfur-free Codonopsis Radix Decoction Pieces from five producing areas were determined by TLC and GC. Heavy metals, harmful elements and pesticide residues were detected by atomic absorption spectrophotometry and GC. The method for content determination of Lobetyolin in Codonopsis Radix was established by HPLC. Results Safety index check items of 21 batches of Codonopsis Radix Decoction Pieces showed: Sulfur dioxide residue ≤ 7 mg/kg, Pb content ≤ 1.124 mg/kg, As content ≤ 0.067 mg/kg, Cd content ≤ 0.058 mg/kg, Hg content ≤ 0.003 mg/kg, Cu content ≤ 14.121 mg/kg. total BHC ≤ 0.03 mg/kg, total DDT ≤ 0.031 mg/kg, and pentachloronitrobenzene(PCNB) ≤ 0.008 mg/kg. The average sample recovery rate of Lobetyolin content was 97.71%, RSD was 1.32%, and the average fraction was 0.138%. Conclusion The safety index of sulfur-free Codonopsis Radix Decoction Pieces is sulfur dioxide residue ≤ 10 mg/kg. The heavy metal and pesticide residue standards meet the limit standard for Codonopsis Radix in pharmacopoeia. The method for determining the effectiveness index is reliable, which can provide a basis for the quality control and clinical use of Codonopsis Radix.
引文
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[13]逄瑜,于新兰,李海芳,等.农药残留测定结果不确定度评定方法指南介绍[J].中国新药杂志,2018,27(1):17-21.
[14]冯佩佩,李忠祥,原忠.党参属药用植物化学成分和药理研究进展[J].沈阳药科大学学报,2012,29(4):307-311.
[2]郭琼琼,李晶,孙海峰,等.党参挥发性成分分析及其特殊香气研究[J].中药材,2016,39(9):2005-2012.
[3]全世佑.浅析党参的加工储藏技术[J].甘肃农业,2013(12):25-26.
[4]吴秋丽,杨晓宾,俞信光,等.中药材原产地无硫加工技术研究进展[J].科技创新导报,2017(32):79-80,82.
[5]张丽芬,戴晖.高效液相色谱法测定党参中党参多糖、党参炔苷的含量[J].临床合理用药杂志,2016,9(28):91-92.
[6] KANG C, LAIC J, ZHAO D, etal. Apractical protocol for comprehensive evaluation of sulfur-fumigation of Gastrodia Rhizoma using metabolome and health risk assessment analysis[J].J Hazard Mater,2017,340:221-230.
[7] DUAN S M, XU J, BAI Y J, et al. Sulfur dioxide residue in sulfur-fumigated edible herbs:The fewer, the safer?[J]. Food Chemistry,2016,192:119-124.
[8]段金廒,赵润怀,宿树兰,等.对硫磺熏蒸药材的基本认识与建议[J].中国现代中药,2011,13(4):3-5,14.
[9]Codex Alimentarius Commission.CODEXSTAN1-1985General standard for the labelling of prepackaged foods(Adopted 1985.Amended 1991, 1999, 2001, 2003, 2005, 2008 and 2010.)[EB/OL].[2018-03-05].http://down.foodmate.net/standard/sort/11/3324.html.
[10] LIU S H, CHUANG W C, LAM W, et al. Safety surveillance of traditional Chinese medicine:current and future[J]. Drug Safety,2015,38(2):117-128.
[11]郭兰萍,周利,王升,等.《中医药中药材重金属限量中药材重金属限量》ISO国际标准下中药材重金属污染现状与分析[J].科技导报,2017,35(11):91-98.
[12]黄靖雯,南铁贵,袁媛,等.中药材质量基本数据探索研究——农药残留分析[J].中国实验方剂学杂志,2017,23(24):56-61.
[13]逄瑜,于新兰,李海芳,等.农药残留测定结果不确定度评定方法指南介绍[J].中国新药杂志,2018,27(1):17-21.
[14]冯佩佩,李忠祥,原忠.党参属药用植物化学成分和药理研究进展[J].沈阳药科大学学报,2012,29(4):307-311.