QuEChERS结合GC-MS/MS-内标法测定川麦冬中多效唑残留量
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摘要
目的:建立测定川麦冬中多效唑残留量的方法,并用于检验不同来源的川麦冬药材质量。方法:收集50批不同产地、市场和企业来源的川麦冬样品,样品前处理方法为QuEChERS法,即样品加水经乙腈提取,以QuEChERS提取包(含无水硫酸镁与无水乙酸钠等)进行盐析,提取液再经QuEChERS净化包(含无水硫酸镁、N-丙基乙二胺、十八烷基硅烷键合硅胶、硅胶、石墨化炭黑)净化后加入内标磷酸三苯酯,采用气相色谱-质谱/质谱联用(GC-MS/MS)法测定川麦冬样品中多效唑残留量。色谱柱为DB-5MS,程序升温,检测器为三重四级杆质谱,载气初始流速为1.3 mL/min,采集方式为多反应监测,不分流进样。结果:多效唑检测质量浓度线性范围为1.01～505 ng/mL(r=0.999 7),精密度试验、稳定性试验(24 h)、重复性试验的RSD分别为3.94%、13.62%、7.54%(n=6),方法回收率平均值为111.26%(RSD=5.43%,n=9);在50批样品中的多效唑检测结果为0.02～2.72 mg/kg。结论:建立的多效唑检测方法操作简便、结果准确、灵敏度及重复性好,可用于川麦冬中多效唑残留量的检测;不同来源的川麦冬样品中多效唑残留量相差较大。
OBJECTIVE:To establish a method for measuring the paclobutrazol residue in Ophiopogon japonicus from Sichuan and detect the quality of O.japonicus from Sichuan from different sources.METHODS:Totally 50 batches of samples were collected from different origin places,commercial markets and manufacturers.The sample pretreatment method was QuEChERS method,.ie the sample was extracted by aqueous acetonitrile,salted out by QuEChERS extract package(containing anhydrous magnesium sulfate and anhydrous sodium acetate),the extract solution was purified by QuEChERS purification package(containing anhydrous magnesium sulfate,N-propyl ethylenediamine,octadecylsilane chemically bonded silica,silica gel,graphitized carbon black)and then added into internal standard triphenyl phosphate.The paclobutrazol residue in O.japonicus from Sichuan was determined by GC-MS/MS.The determination was performed on DB-5MS column.The temperature programming was adopted,and the detector was triple quadrupole MS detector.The initial flow rate of carrier gas was 1.3 m L/min;acquisition mode was MRM.Injection method was splitless injection.RESULTS:The linear range of paclobutrazol was 1.01-505 ng/mL(r=0.999 7).RSDs of precision,stability(24 h)and repeatability tests were 3.94%,13.62%,7.54%(n=6),respectively.Average method recovery was 111.26%(RSD=5.43%,n=9).The paclobutrazol residue in 50 batches of sample were 0.02-2.72 mg/kg.CONCLUSIONS:Established method is simple,accurate,sensitive and reproducible.It also can be used for the determination of paclobutrazol residue in O.japonicus from Sichuan.The contents of paclobutrazol residue in O.japonicus from Sichuan from different sources are different greatly.
OBJECTIVE:To establish a method for measuring the paclobutrazol residue in Ophiopogon japonicus from Sichuan and detect the quality of O.japonicus from Sichuan from different sources.METHODS:Totally 50 batches of samples were collected from different origin places,commercial markets and manufacturers.The sample pretreatment method was QuEChERS method,.ie the sample was extracted by aqueous acetonitrile,salted out by QuEChERS extract package(containing anhydrous magnesium sulfate and anhydrous sodium acetate),the extract solution was purified by QuEChERS purification package(containing anhydrous magnesium sulfate,N-propyl ethylenediamine,octadecylsilane chemically bonded silica,silica gel,graphitized carbon black)and then added into internal standard triphenyl phosphate.The paclobutrazol residue in O.japonicus from Sichuan was determined by GC-MS/MS.The determination was performed on DB-5MS column.The temperature programming was adopted,and the detector was triple quadrupole MS detector.The initial flow rate of carrier gas was 1.3 m L/min;acquisition mode was MRM.Injection method was splitless injection.RESULTS:The linear range of paclobutrazol was 1.01-505 ng/mL(r=0.999 7).RSDs of precision,stability(24 h)and repeatability tests were 3.94%,13.62%,7.54%(n=6),respectively.Average method recovery was 111.26%(RSD=5.43%,n=9).The paclobutrazol residue in 50 batches of sample were 0.02-2.72 mg/kg.CONCLUSIONS:Established method is simple,accurate,sensitive and reproducible.It also can be used for the determination of paclobutrazol residue in O.japonicus from Sichuan.The contents of paclobutrazol residue in O.japonicus from Sichuan from different sources are different greatly.
引文
[1]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:155-156.
[2]胥秀英,郑一敏,傅善权,等.HPLC法同时测定麦冬药材中麦冬皂苷Ra和慈溪麦冬皂苷A的含量[J].中国药房,2010,21(39):3704-3705.
[3]包小红,苟琰,魏伯平,等.麦冬中外源性有害物质的分析[J].中成药,2017,39(9):1969-1971.
[4]贾洪涛.植物生长延缓剂:多效唑[J].农技服务,2004(1):60-61.
[5]SCHENCK FJ,HOBBS JE.Evaluation of the quick,easy,cheap,effective,rugged,and safe(QuEChERS)approach to pesticide residue analysis[J].Bull Environ Contam Toxicol,2004,73(1):24-30.
[6]董静,潘玉香,朱莉萍,等.果蔬中54种农药残留的QuEChERS/GC-MS快速分析[J].分析测试学报,2008,27(1):66-69.
[7]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京:中国医药科技出版社,2015:212-224.
[8]林秋霞,李敏,罗远鸿,等.植物生长调节剂对川麦冬生长发育影响的研究[J].时珍国医国药,2014,25(8):1994-1996.
[9]林秋霞,李敏,周海玉,等.植物生长调节剂对川麦冬总皂苷和总多糖含量的影响研究[J].中国现代中药,2014,16(5):399-401,409.
[10]何瑞,刘艾平,曹玉广.植物生长调节剂使用中的安全问题[J].中国卫生监督杂志,2003,10(2):99-101.
[11]包媛媛,张新永,邵金良.多效唑在番茄和土壤中的残留与降解动态研究[J].生态环境学报,2014,23(5):864-869.
[12]国家卫生和计划生育委员会,农业部,国家食品药品监督管理总局.食品中农药最大残留限量GB-2763-2016[S].2016-12-18.
[13]徐国锋,聂继云,李静,等.GC/ECD测定葡萄中多效唑和烯效唑的残留[J].农药,2014,53(10):736-738,755.
[14]吕燕,赵健,杨挺,等.气相色谱质谱法检测蔬菜中多效唑的残留[J].中国测试,2010,36(4):57-59.
[15]黄琦,黄战威,陈振威,等.气相色谱-质谱法快速检测芒果园土壤中多效唑[J].南方农业学报,2015,46(6):1042-1046.
[16]孙星,丁悦,汪佳蕾,等.QuEChERS-高效液相色谱-串联质谱法测定果蔬中多效唑残留[J].食品科学,2014,35(8):76-79.
[17]张敏,闫超杰,付海滨,等.固相萃取净化-高效液相色谱测定水果中赤霉素、多效唑、烯效唑残留量[J].食品与发酵工业,2014,40(2):192-195.
[18]宋莹,张耀海,黄霞,等.气相色谱-串联质谱法快速检测水果中的多效唑残留[J].分析化学,2011,39(8):1270-1273.
[19]翟宇瑶,郭宝林.高效液相色谱-串联质谱测定4种植物生长延缓剂在6种根及根茎类药材中残留量[J].中国中药杂志,2017,42(11):2110-2116.
[20]杨言琛,张兴国,郝安辉,等.HPLC法测定麦冬及环境中多效唑的残留量[J].西部中医药,2016,29(9):37-39.
[21]林秋霞.植物生长调节剂对川麦冬质量的影响研究[D]成都:成都中医药大学,2014.
[22]苟琰,耿昭,吴强,等.气相色谱-串联质谱法检测麦冬中农药残留[J].中国药学杂志,2018,53(7):555-560.
[2]胥秀英,郑一敏,傅善权,等.HPLC法同时测定麦冬药材中麦冬皂苷Ra和慈溪麦冬皂苷A的含量[J].中国药房,2010,21(39):3704-3705.
[3]包小红,苟琰,魏伯平,等.麦冬中外源性有害物质的分析[J].中成药,2017,39(9):1969-1971.
[4]贾洪涛.植物生长延缓剂:多效唑[J].农技服务,2004(1):60-61.
[5]SCHENCK FJ,HOBBS JE.Evaluation of the quick,easy,cheap,effective,rugged,and safe(QuEChERS)approach to pesticide residue analysis[J].Bull Environ Contam Toxicol,2004,73(1):24-30.
[6]董静,潘玉香,朱莉萍,等.果蔬中54种农药残留的QuEChERS/GC-MS快速分析[J].分析测试学报,2008,27(1):66-69.
[7]国家药典委员会.中华人民共和国药典:四部[S].2015年版.北京:中国医药科技出版社,2015:212-224.
[8]林秋霞,李敏,罗远鸿,等.植物生长调节剂对川麦冬生长发育影响的研究[J].时珍国医国药,2014,25(8):1994-1996.
[9]林秋霞,李敏,周海玉,等.植物生长调节剂对川麦冬总皂苷和总多糖含量的影响研究[J].中国现代中药,2014,16(5):399-401,409.
[10]何瑞,刘艾平,曹玉广.植物生长调节剂使用中的安全问题[J].中国卫生监督杂志,2003,10(2):99-101.
[11]包媛媛,张新永,邵金良.多效唑在番茄和土壤中的残留与降解动态研究[J].生态环境学报,2014,23(5):864-869.
[12]国家卫生和计划生育委员会,农业部,国家食品药品监督管理总局.食品中农药最大残留限量GB-2763-2016[S].2016-12-18.
[13]徐国锋,聂继云,李静,等.GC/ECD测定葡萄中多效唑和烯效唑的残留[J].农药,2014,53(10):736-738,755.
[14]吕燕,赵健,杨挺,等.气相色谱质谱法检测蔬菜中多效唑的残留[J].中国测试,2010,36(4):57-59.
[15]黄琦,黄战威,陈振威,等.气相色谱-质谱法快速检测芒果园土壤中多效唑[J].南方农业学报,2015,46(6):1042-1046.
[16]孙星,丁悦,汪佳蕾,等.QuEChERS-高效液相色谱-串联质谱法测定果蔬中多效唑残留[J].食品科学,2014,35(8):76-79.
[17]张敏,闫超杰,付海滨,等.固相萃取净化-高效液相色谱测定水果中赤霉素、多效唑、烯效唑残留量[J].食品与发酵工业,2014,40(2):192-195.
[18]宋莹,张耀海,黄霞,等.气相色谱-串联质谱法快速检测水果中的多效唑残留[J].分析化学,2011,39(8):1270-1273.
[19]翟宇瑶,郭宝林.高效液相色谱-串联质谱测定4种植物生长延缓剂在6种根及根茎类药材中残留量[J].中国中药杂志,2017,42(11):2110-2116.
[20]杨言琛,张兴国,郝安辉,等.HPLC法测定麦冬及环境中多效唑的残留量[J].西部中医药,2016,29(9):37-39.
[21]林秋霞.植物生长调节剂对川麦冬质量的影响研究[D]成都:成都中医药大学,2014.
[22]苟琰,耿昭,吴强,等.气相色谱-串联质谱法检测麦冬中农药残留[J].中国药学杂志,2018,53(7):555-560.