色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
1期
75-79
,共5页
周晓%李小兰%陈志燕%叶长文%周芸%孟冬玲
週曉%李小蘭%陳誌燕%葉長文%週蕓%孟鼕玲
주효%리소란%진지연%협장문%주예%맹동령
高效液相色谱%异噻唑啉酮类杀菌剂%水基胶黏剂
高效液相色譜%異噻唑啉酮類殺菌劑%水基膠黏劑
고효액상색보%이새서람동류살균제%수기효점제
high performance liquid chromatography( HPLC)%isothiazolone biocides%water-borne adhesives
建立了一种高效液相色谱法快速测定水基胶黏剂中3种异噻唑啉酮类杀菌剂(2-甲基-4-异噻唑啉-3-酮(MI)、5-氯-2-甲基-4-异噻唑啉-3-酮(CMI)和1,2-苯并异噻啉-3-酮(BIT))的分析方法。样品经甲醇-水(1:1,v/v)溶液振荡提取、离心、过滤后,采用高效液相色谱-二极管阵列检测器检测,C18色谱柱分离,流动相为甲醇-水,梯度洗脱。对前处理条件(包括萃取溶剂、提取方式、稀释倍数、提取时间)进行了优化。在优化实验条件下,样品中的异噻唑啉酮在0.25~10.0 mg/L范围内呈良好的线性关系( r2≥0.9992),加标回收率在92%~103%之间,相对标准偏差不高于4%,检出限为0.43~1.14 mg/kg,定量限为1.44~3.81 mg/kg。结果表明该方法能达到定量检测的目的。将该方法应用于实际样品的检测,结果可靠。
建立瞭一種高效液相色譜法快速測定水基膠黏劑中3種異噻唑啉酮類殺菌劑(2-甲基-4-異噻唑啉-3-酮(MI)、5-氯-2-甲基-4-異噻唑啉-3-酮(CMI)和1,2-苯併異噻啉-3-酮(BIT))的分析方法。樣品經甲醇-水(1:1,v/v)溶液振盪提取、離心、過濾後,採用高效液相色譜-二極管陣列檢測器檢測,C18色譜柱分離,流動相為甲醇-水,梯度洗脫。對前處理條件(包括萃取溶劑、提取方式、稀釋倍數、提取時間)進行瞭優化。在優化實驗條件下,樣品中的異噻唑啉酮在0.25~10.0 mg/L範圍內呈良好的線性關繫( r2≥0.9992),加標迴收率在92%~103%之間,相對標準偏差不高于4%,檢齣限為0.43~1.14 mg/kg,定量限為1.44~3.81 mg/kg。結果錶明該方法能達到定量檢測的目的。將該方法應用于實際樣品的檢測,結果可靠。
건립료일충고효액상색보법쾌속측정수기효점제중3충이새서람동류살균제(2-갑기-4-이새서람-3-동(MI)、5-록-2-갑기-4-이새서람-3-동(CMI)화1,2-분병이새람-3-동(BIT))적분석방법。양품경갑순-수(1:1,v/v)용액진탕제취、리심、과려후,채용고효액상색보-이겁관진렬검측기검측,C18색보주분리,류동상위갑순-수,제도세탈。대전처리조건(포괄췌취용제、제취방식、희석배수、제취시간)진행료우화。재우화실험조건하,양품중적이새서람동재0.25~10.0 mg/L범위내정량호적선성관계( r2≥0.9992),가표회수솔재92%~103%지간,상대표준편차불고우4%,검출한위0.43~1.14 mg/kg,정량한위1.44~3.81 mg/kg。결과표명해방법능체도정량검측적목적。장해방법응용우실제양품적검측,결과가고。
A rapid high performance liquid chromatography( HPLC)method was developed for the quantitative analysis of three isothiazolinone biocides( 2-methyl-4-isothiazolin-3-one( MI), 5-chloro-2-methyl-4-isothiazolin-3-one ( CMI ) and 1,2-benzylisothiazolin-3-one ( BIT )) in water-borne adhesives. The sample was extracted with methanol-water(1:1,v/v),and puri-fied by centrifugation and filtration. The isothiazolones were separated on a C18 column with methanol-water as mobile phases under gradient elution and detected with a diode array detector( DAD). The pretreatment factors such as extraction solvent,extraction method,dilu-tion ratio,extraction time were optimized. Under the optimized conditions,the targets had good linearities( r2≥0. 999 2)in the range of 0. 25-10. 0 mg/L. The recoveries were between 92% and 103% with the relative standard deviations not more than 4%. The limits of detection ( LODs)were between 0. 43 mg/kg and 1. 14 mg/kg. The limits of quantification( LOQs)were between 1. 44 mg/kg and 3. 81 mg/kg. The results showed that the method can achieve the pur-pose of quantitative detection. The analyses of real samples verified the reliability of this method.