生物加工过程
生物加工過程
생물가공과정
CHINESE JOURNAL OF BIOPROCESS ENGINEERING
2014年
3期
69-72
,共4页
方芳%魏荣卿%刘晓宁%李寿椿
方芳%魏榮卿%劉曉寧%李壽椿
방방%위영경%류효저%리수춘
衍生%2,5 二甲氧基苯磺酰氯%草甘膦%高效液相色谱
衍生%2,5 二甲氧基苯磺酰氯%草甘膦%高效液相色譜
연생%2,5 이갑양기분광선록%초감련%고효액상색보
derivatization%2,5-dimethoxybenzenesulfonyl chloride%glyphosate%HPLC
以2,5二甲氧基苯磺酰氯( DMOSC)为柱前衍生化试剂,建立了柱前衍生草甘膦的紫外检测反相高效液相色谱法,并优化了衍生化条件,得最佳条件:衍生温度35℃,时间15 min, pH 10?0,草甘膦与DMOSC的摩尔比为1∶6。HPLC分析条件:采用Kromasil C18柱,流速1?0 mL/min,柱温30℃,检测波长220 nm,流动相为甲醇-乙腈-磷酸盐缓冲溶液(0?02 mol/L、pH 5?5),三者的体积比为15∶5∶80。结果表明:草甘膦质量浓度在5~100μg/mL范围内线性关系良好,相关系数为0?9962,检测限为0?067μg/mL。实验表明该方法反应条件温和,灵敏度高,衍生产物稳定。
以2,5二甲氧基苯磺酰氯( DMOSC)為柱前衍生化試劑,建立瞭柱前衍生草甘膦的紫外檢測反相高效液相色譜法,併優化瞭衍生化條件,得最佳條件:衍生溫度35℃,時間15 min, pH 10?0,草甘膦與DMOSC的摩爾比為1∶6。HPLC分析條件:採用Kromasil C18柱,流速1?0 mL/min,柱溫30℃,檢測波長220 nm,流動相為甲醇-乙腈-燐痠鹽緩遲溶液(0?02 mol/L、pH 5?5),三者的體積比為15∶5∶80。結果錶明:草甘膦質量濃度在5~100μg/mL範圍內線性關繫良好,相關繫數為0?9962,檢測限為0?067μg/mL。實驗錶明該方法反應條件溫和,靈敏度高,衍生產物穩定。
이2,5이갑양기분광선록( DMOSC)위주전연생화시제,건립료주전연생초감련적자외검측반상고효액상색보법,병우화료연생화조건,득최가조건:연생온도35℃,시간15 min, pH 10?0,초감련여DMOSC적마이비위1∶6。HPLC분석조건:채용Kromasil C18주,류속1?0 mL/min,주온30℃,검측파장220 nm,류동상위갑순-을정-린산염완충용액(0?02 mol/L、pH 5?5),삼자적체적비위15∶5∶80。결과표명:초감련질량농도재5~100μg/mL범위내선성관계량호,상관계수위0?9962,검측한위0?067μg/mL。실험표명해방법반응조건온화,령민도고,연생산물은정。
A derivatization method for the determination of glyphosate had been developed by using 2,5-dimethoxybenzenesulfonyl chloride?The optimized conditions of derivatization were as follows:reaction temperature 35 ℃,reaction time 15 min,solution pH value 10?0,the buffer reaction concentration 0?2 mol/L,and ratio of n( glyphosate) ∶n( o-nitrobenzenesulfonyl)= 1∶6?The chromatographic conditions were as follows:Kromasil C18 column(5 μm,4?6 ×250 mm),detection wavelength 220 nm,flow rate 1?0 mL/min,mobile phase A ( methanol)∶mobile phase B ( acetonitrile)∶mobile phase C ( phosphate buffer solution(PBS,pH 5?5,0?02 mol/L))= 15∶5∶80,isocratic elution.The calibration curve for glyphosate was linear ranging from 5 μg/mL to 100 μg/mL. The linear correlation coefficient was 0?996 2. The limit of detection was 0?067 μg/mL?The experimental result shows that the method is simple,rapid and reliable,and generally applicable.