篇名: QuEChERS结合GC-MS/MS-内标法测定川麦冬中多效唑残留量
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。
ABSTRACT: 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 mL/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.
期刊: 2019年第30卷第3期
作者: 苟琰,高驰,邓晶晶,李红彦,耿昭,周娟,袁军,李敏
AUTHORS: GOU Yan,GAO Chi,DENG Jingjing,LI Hongyan,GENG Zhao,ZHOU Juan,YUAN Jun,LI Min
关键字: 川麦冬;气相色谱-质谱/质谱联用法;内标;多效唑;残留量
KEYWORDS: Ophiopogon japonicus from Sichuan; GC-MS/MS; Internal standard; Paclobutrazol; Residue
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