色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
8期
849-855
,共7页
在线固相微萃取%高效液相色谱%苯氧羧酸类除草剂%整体柱%同步富集检测
在線固相微萃取%高效液相色譜%苯氧羧痠類除草劑%整體柱%同步富集檢測
재선고상미췌취%고효액상색보%분양최산류제초제%정체주%동보부집검측
on-line solid phase microextraction%high performance liquid chromatography(HPLC)%phenoxy acid herbicides%monolithic column%synchronous extraction and determination
采用 C18毛细管整体柱作为固相微萃取整体柱，构建在线固相微萃取-高效液相色谱联用系统，同步富集检测环境水样中的5种苯氧羧酸类除草剂。详细考察了联用系统运行条件对富集检测的影响。联用系统运行最佳参数为：固相微萃取整体柱长度20 cm，进样流速0.04 mL／min，进样13 min，洗脱流速0.02 mL／min，洗脱5 min。在最佳条件下，5种苯氧羧酸类除草剂的检出限为：9μg／L（苯氧丙酸）、4μg／L（2-（2-氯）-苯氧丙酸）、4μg／L（2-（3-氯）-苯氧丙酸）、5μg／L（2，4-二氯苯氧乙酸）、5μg／L（2-（2，4-二氯苯氧基）丙酸）。与 HPLC 系统直接进样对比，联用系统对5种检测对象表现出优良的富集能力。5种苯氧羧酸类除草剂的回收率在79.0％~98.0％之间（ RSD≤3.9％）。该方法成功应用于水样中5种苯氧羧酸类除草剂的检测，结果令人满意。
採用 C18毛細管整體柱作為固相微萃取整體柱，構建在線固相微萃取-高效液相色譜聯用繫統，同步富集檢測環境水樣中的5種苯氧羧痠類除草劑。詳細攷察瞭聯用繫統運行條件對富集檢測的影響。聯用繫統運行最佳參數為：固相微萃取整體柱長度20 cm，進樣流速0.04 mL／min，進樣13 min，洗脫流速0.02 mL／min，洗脫5 min。在最佳條件下，5種苯氧羧痠類除草劑的檢齣限為：9μg／L（苯氧丙痠）、4μg／L（2-（2-氯）-苯氧丙痠）、4μg／L（2-（3-氯）-苯氧丙痠）、5μg／L（2，4-二氯苯氧乙痠）、5μg／L（2-（2，4-二氯苯氧基）丙痠）。與 HPLC 繫統直接進樣對比，聯用繫統對5種檢測對象錶現齣優良的富集能力。5種苯氧羧痠類除草劑的迴收率在79.0％~98.0％之間（ RSD≤3.9％）。該方法成功應用于水樣中5種苯氧羧痠類除草劑的檢測，結果令人滿意。
채용 C18모세관정체주작위고상미췌취정체주，구건재선고상미췌취-고효액상색보련용계통，동보부집검측배경수양중적5충분양최산류제초제。상세고찰료련용계통운행조건대부집검측적영향。련용계통운행최가삼수위：고상미췌취정체주장도20 cm，진양류속0.04 mL／min，진양13 min，세탈류속0.02 mL／min，세탈5 min。재최가조건하，5충분양최산류제초제적검출한위：9μg／L（분양병산）、4μg／L（2-（2-록）-분양병산）、4μg／L（2-（3-록）-분양병산）、5μg／L（2，4-이록분양을산）、5μg／L（2-（2，4-이록분양기）병산）。여 HPLC 계통직접진양대비，련용계통대5충검측대상표현출우량적부집능력。5충분양최산류제초제적회수솔재79.0％~98.0％지간（ RSD≤3.9％）。해방법성공응용우수양중5충분양최산류제초제적검측，결과령인만의。
A C18 monolithic capillary column was utilized as the solid phase microextraction column to construct an in-tube SPME-HPLC system which was used to simultaneously extract and detect five phenoxy acid herbicides,including 2,4-dichlorophenoxyacetic acid(2,4-D),2-(2-chloro)-phenoxy propionic acid(2,2-CPPA),2-(3-chloro)-phenoxy propionic acid(2,3-CPPA),phenoxy propionic acid(PPA)and 2-(2,4-dichlorophenoxy)propionic acid(2,4-DP). The operating parameters of the in-tube SPME-HPLC system ,including the length of the mono-lithic column,the sampling flow rate,the sampling time,the elution flow rate and the elution time,had been investigated in detail. The optimized operating parameters of the in-tube SPME-HPLC system were as follow:the length of the monolithic column was 20 cm,the sampling flow rate was 0. 04 mL/min, sampling time was 13 min;the elution flow rate was 0. 02 mL/min,elution time was 5 min. Under the optimized conditions,the detection limits of the five phenoxy acid herbicides were as follows:9 μg/L for PPA,4 μg/L for 2,2-CPPA,4 μg/L for 2,3-CPPA,5 μg/L for 2,4-D,5 μg/L for 2,4-DP. Compared with the HPLC method with di-rect injection,the combined system showed a good enrichment factors to the analytes. The re-coveries of the five phenoxy acid herbicides were between 79. 0% and 98. 0%( RSD≤3. 9%). This method was successfully used to detect the five phenoxy acid herbicides in water samples with satisfactory results.
