分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
8期
1178-1183
,共6页
何红梅%张春荣%朱亚红%张昌朋%平立凤%赵华%吴珉%汤涛%蔡晓明%李振
何紅梅%張春榮%硃亞紅%張昌朋%平立鳳%趙華%吳珉%湯濤%蔡曉明%李振
하홍매%장춘영%주아홍%장창붕%평립봉%조화%오민%탕도%채효명%리진
溴氰虫酰胺%J9Z38%辣椒%残留%液相色谱-串联质谱
溴氰蟲酰胺%J9Z38%辣椒%殘留%液相色譜-串聯質譜
추청충선알%J9Z38%랄초%잔류%액상색보-천련질보
Cyantraniliprole%J9 Z38%Pepper%Residue%Ultra performance liquid chromatography-tandem mass spectrometry
建立了超高效液相色谱-串联质谱法( UPLC-MS/MS )测定辣椒和土壤中溴氰虫酰胺及其代谢物(J9Z38)残留量的方法,研究了溴氰虫酰胺和J9Z38在辣椒和土壤上的降解特性。样品经乙腈提取后用C18固相萃取柱净化,采用梯度洗脱程序、BEH C18色谱分离柱、应用UPLC-MS/MS正离子扫描测定溴氰虫酰胺和J9Z38。进行了添加浓度为0.01、0.10和1.00 mg/kg的回收实验,溴氰虫酰胺和J9Z38在辣椒和土壤中的日内平均回收率为88.6%~105.7%,日内相对标准偏差为3.8%~15.1%；日间平均回收率为91.4%~105.3%,日间相对标准偏差为4.9%~12.3%。溴氰虫酰胺和J9Z38在2.0~128.0μg/L浓度范围内相关系数r>0.9992,定量限分别为0.1和0.2μg/kg。应用本方法检测了田间实验样品,结果表明,溴氰虫酰胺在辣椒和土壤中降解半衰期分别为9.2~11.2 d和9.2~20.8 d,J9Z38在辣椒中残留量低于定量限,在土壤中降解半衰期为9.4 d；随着降水量增加,溴氰虫酰胺降解速度加快。
建立瞭超高效液相色譜-串聯質譜法( UPLC-MS/MS )測定辣椒和土壤中溴氰蟲酰胺及其代謝物(J9Z38)殘留量的方法,研究瞭溴氰蟲酰胺和J9Z38在辣椒和土壤上的降解特性。樣品經乙腈提取後用C18固相萃取柱淨化,採用梯度洗脫程序、BEH C18色譜分離柱、應用UPLC-MS/MS正離子掃描測定溴氰蟲酰胺和J9Z38。進行瞭添加濃度為0.01、0.10和1.00 mg/kg的迴收實驗,溴氰蟲酰胺和J9Z38在辣椒和土壤中的日內平均迴收率為88.6%~105.7%,日內相對標準偏差為3.8%~15.1%；日間平均迴收率為91.4%~105.3%,日間相對標準偏差為4.9%~12.3%。溴氰蟲酰胺和J9Z38在2.0~128.0μg/L濃度範圍內相關繫數r>0.9992,定量限分彆為0.1和0.2μg/kg。應用本方法檢測瞭田間實驗樣品,結果錶明,溴氰蟲酰胺在辣椒和土壤中降解半衰期分彆為9.2~11.2 d和9.2~20.8 d,J9Z38在辣椒中殘留量低于定量限,在土壤中降解半衰期為9.4 d；隨著降水量增加,溴氰蟲酰胺降解速度加快。
건립료초고효액상색보-천련질보법( UPLC-MS/MS )측정랄초화토양중추청충선알급기대사물(J9Z38)잔류량적방법,연구료추청충선알화J9Z38재랄초화토양상적강해특성。양품경을정제취후용C18고상췌취주정화,채용제도세탈정서、BEH C18색보분리주、응용UPLC-MS/MS정리자소묘측정추청충선알화J9Z38。진행료첨가농도위0.01、0.10화1.00 mg/kg적회수실험,추청충선알화J9Z38재랄초화토양중적일내평균회수솔위88.6%~105.7%,일내상대표준편차위3.8%~15.1%；일간평균회수솔위91.4%~105.3%,일간상대표준편차위4.9%~12.3%。추청충선알화J9Z38재2.0~128.0μg/L농도범위내상관계수r>0.9992,정량한분별위0.1화0.2μg/kg。응용본방법검측료전간실험양품,결과표명,추청충선알재랄초화토양중강해반쇠기분별위9.2~11.2 d화9.2~20.8 d,J9Z38재랄초중잔류량저우정량한,재토양중강해반쇠기위9.4 d；수착강수량증가,추청충선알강해속도가쾌。
An analytical method based on ultra performance liquid chromatography-tandem mass spectrometry was developed for the determination of cyantraniliprole and its main metabolite J9 Z38 residues in pepper and soil. The fate of cyantraniliprole and J9Z38 in pepper and soil was also evaluated. The target compounds were extracted with acetonitrile, cleaned up by C18 cartridge, and further analyzed by gradient ultra performance liquid chromatography-tandem mass spectrometry with electrospray ionization in positive mode ( ESI﹢) using a UPLC BEH C18 Column. The method was validated using fortified pepper and soil. Intra-day mean recoveries of cyantraniliprole and J9Z38 at three spiked levels (0. 01, 0. 10 and 1. 00 mg/kg) ranged from 88. 6% to 105 . 7% with relative standard deviations of 3 . 8%-15 . 1%. Inter-day mean recoveries of cyantraniliprole and J9 Z38 were found between 91 . 4% and 105 . 3% with relative standard deviations of 4 . 9%-12 . 3% at three spiked levels. Limits of quantification ( LOQs) of cyantraniliprole and J9Z38 were 0. 1 and 0. 2 μg/kg, respectively. Linear calibration functions with correlation coefficients of r>0. 9992 were obtained in the concentration range of 2. 0-128. 0 μg/L. This method was applied to the analysis of cyantraniliprole and J9Z38 residues in real pepper and soil samples selected from field. The results of the residue dynamic experiment showed that the half-life of cyantraniliprole ranged from 9 . 2 to 11 . 2 days in pepper and from 9 . 2 to 20. 8 days in soil. While, the residues of J9Z38 in pepper were below LOQ, and the half-life of J9Z38 in soil was 9. 4 days. The degradation speed of cyantraniliprole increased with the increase of the precipitation.
