高效液相色譜-串聯(lián)質(zhì)譜測定4種植物生長延緩劑在6種根及根莖類藥材中殘留量
發(fā)布時間:2018-04-29 18:57
本文選題:高效液相色譜-串聯(lián)質(zhì)譜法 + 根類藥材 ; 參考:《中國中藥雜志》2017年11期
【摘要】:建立了適用于根及根莖類藥材中同時測定多效唑、丁酰肼、矮壯素和縮節(jié)胺4種植物生長延緩劑殘留量的高效液相色譜-串聯(lián)質(zhì)譜(HPLC-MS-MS)測定方法。根類藥材樣品分別經(jīng)含0.1%甲酸的乙腈混合液提取兩次,混合提取溶液經(jīng)Waters Atlantis HILIC色譜柱(2.1 mm×150 mm,3.0μm)分離,用含0.1%甲酸的0.005 mol·L~(-1)醋酸銨溶液-甲醇-乙腈(13∶15∶72)等度洗脫,采用電噴霧正離子模式多反應(yīng)監(jiān)測。4種植物生長延緩劑在6~1 500μg·kg~(-1)線性良好,相關(guān)系數(shù)為0.997 8~0.999 9;加樣回收率為79.3%~103.3%,相對標(biāo)準(zhǔn)偏差(RSD)均不大于11%。在檢測的麥冬、當(dāng)歸、牛膝、澤瀉、川芎和三七等藥材中,4種植物生長延緩劑在其中部分藥材中有檢出,其中較為嚴(yán)重的情況是,麥冬的多效唑檢測量為63.4~1 351.6μg·kg~(-1),麥冬、澤瀉、川芎、當(dāng)歸4種藥材中檢測到丁酰肼。
[Abstract]:A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) method was developed for the simultaneous determination of four plant growth retardants, paclobutrazol, butyric hydrazide, dwarf and acylamine, in root and rhizome herbs. The root medicinal materials were extracted twice by acetonitrile mixture containing 0.1% formic acid. The mixed extraction solution was separated by Waters Atlantis HILIC chromatographic column (2.1mm 脳 150mm) and eluted with 0.005 mol L ~ (-1) (containing 0.1% formic acid) ammonium acetate solution-methanol-acetonitrile (13: 15: 72). The linear range of 4 plant growth retardants was 0.997 渭 g / kg ~ (-1), the correlation coefficient was 0.997 ~ (0.999 9), the recovery rate was 79.3% and the relative standard deviation (RSD) was less than 11 ~ (-1). Four plant growth retardants, such as Radix Ophiopogonis, Radix angelicae Sinensis, Radix Achyranthes bidentata, Radix Alismatis, Ligusticum chuanxiong and Radix Notoginseng, were detected in some of them. Butyric hydrazide was detected in 4 kinds of medicinal materials of Ligusticum chuanxiong and Angelica sinensis.
【作者單位】: 中國醫(yī)學(xué)科學(xué)院北京協(xié)和醫(yī)學(xué)院藥用植物研究所;西安市第四醫(yī)院;
【分類號】:O657.63;R284.1
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