| ObjectiveIn recent years,the health of traditional Chinese medicine has been promoted to the level of national strategy.The industry of traditional Chinese medicine has shown a trend of rapid development.However,pesticide residues and control technology have become an important restrictive factor for the quality assurance of traditional Chinese medicine,which is related to the healthy development of the industry chain of traditional Chinese medicine,and is also one of the key problems to be solved urgently in the development of the industry of traditional Chinese medicine.At present,there are not many methods and limits for the determination of pesticide residues in traditional Chinese medicines.In the 2015 edition of the Chinese Pharmacopoeia,only 19 organochlorine pesticides residues in four kinds of traditional Chinese medicines are limited.Pretreatment technology is the main factor affecting the accuracy and efficiency of pesticide residues detection.Through the research,this experiment intends to establish a rapid,efficient and accurate pre-treatment technology for the detection of pesticide residues in different kinds of traditional Chinese medicines,and optimize the establishment of an instrument for simultaneous detection of multiple pesticides,in order to provide an efficient and accurate method for the detection of pesticide residues in traditional Chinese medicines.It also provides a reference for strengthening the establishment of relevant limit standards for the detection of pesticide residues in traditional Chinese medicines and the quality control of traditional Chinese medicines.MethodsThis study systematically investigated and optimized the factors such as extractant and purifier in the detection of different kinds of Chinese medicinal herbs by QuEChERS sample pretreatment technology,and optimized the temperature-rising procedure and collision energy of the instrument method.Taking Panax notoginseng as the representative of root and rhizome medicines,a rapid and simultaneous determination method of 18 organophosphorus pesticides(Sulfotep,Phorate,Terbufos,Fonofos,Diazinon,Disulfoton,Dichlofenthion,Fenchlorphos,Pirimiphos-methyl,Malathion,Isocarbophos,Trichloronate,Bromophos,Quinalphos,Methidathion,Ditalimfos,Ethion,Triazophos)residues by QuEChERS-GC-MS/MS was established.Meanwhile,negative labeling tests were carried out with samples of Panax notoginseng,Chonglou,Gastrodia elata and Rhubarb in several batches.A QuEChERS-GC-MS/MS method was established for the rapid and simultaneous determination of nine organophosphorus pesticides(Sulfotep,Terbufos,Disulfoton,Fenchlorphos,Malathion,Isocarbophos,Bromophos,Quinalphos,Triazophos)residues in flower medicines.Several batches of safflower and honeysuckle were used as samples.To establish QuEChERS-GC-MS/MS for rapid and simultaneous determination of nine organophosphorus insecticides and fungicides(Phorate,Fonofos,Diazinon,Dichlofenthion,Pirimiphos-methyl,Trichloronate,Methidathion,Ditalimfos,Ethion,)residues in fruits of Schisandra chinensis as the representative of fruits,and then take several batches of Schisandra chinensis and Xanthium sibiricum as samples.Negative labeling was performed by the established method.At the same time,the linearity,precision,recovery rate,detection limit and quantitative limit of each method were investigated.ResultsThe rhizome medicinal materials represented by Panax notoginseng were extracted with15 m L 1% glacial acetic acid-acetonitrile and 0.6 g Mg SO4.0.100 g PSA and 0.100 g C18 were used as purifiers for pretreatment;the linear relationship of 18 organophosphorus pesticides was good in the linear range of 0.025～0.200 ug/m L,and the correlation coefficient(r)was not less than 0.998 0;the detection limit of the method was 5.0～18.75 ug/kg,and the quantitative limit was 9.38～31.25 ug/kg;the average recovery of standard addition was70.21%～140.62%,and RSD was 2.67%～5.22%.Several batches of Panax notoginseng,Gastrodia elata,Rhubarb and Rhubarb were recovered by negative standard addition.The recovery rate was 74.67%～127.48%,RSD value was 0.58%～4.07%.The established method was suitable for the simultaneous,rapid and accurate detection of 18 organophosphorus pesticide residues in this kind of medicinal material.The floral medicinal materials represented by "safflower" were pretreated with acetonitrile at 15 m L,0.6 g MgSO4,0.100 g PSA and 0.050 g GCB as purifiers.The linear relationship of the nine organophosphorus pesticides tested was good in the linear range of0.020～0.120 ug/m L,and the correlation coefficient(r)was not less than 0.999 8.The average recoveries were 99.04%～121.90% and RSD was 0.90%.The detection limit was 5.0～12.50ug/kg and the quantitative limit was 9.38～16.25 ug/kg.The recoveries of negative standard addition of safflower and honeysuckle in several batches were 87.03%～112.08%.The recoveries were good with RSD values of 0.78%～2.57%.The established method can meet the requirements of rapid and accurate detection of the above nine organophosphorus pesticides.Fruit medicines represented by Schisandra chinensis were pretreated with 15 m L 1%glacial acetic acid-acetonitrile as extracting solvent,0.6 g MgSO4,0.100 g PSA and 0.050 g C18 as purifying agent.The linear relationship of nine organophosphorus pesticides and fungicides detected was good in the linear range of 0.020～0.120 ug/m L,and the correlation coefficient(r)was not less than 0.999.The detection limit of the method was 5.0～18.75.The average recovery was 94.14%～124.08% and RSD was 0.66%～1.65%.The recoveries of negative standard addition of Schisandra chinensis and Xanthium sibiricum in several batches were 88.04%～106.26%.The recoveries were good with RSD values of 0.32%～2.15%.The established method can meet the requirements of rapid and accurate detection of the above nine organophosphorus pesticides.ConclusionThe established methods have good linear relationship,high precision and accuracy,and good recovery rate.The optimized pretreatment method has high extraction rate,simplicity,rapidity and cost-saving,which can provide methodological reference for the detection of pesticide residues in Panax Notoginseng and other traditional Chinese medicines. |
PDF Full Text Request