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。
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.
参考文献
[1] | Chen Y C,Xie X B,Shi Q S,et al. Fine and Specialty Chemicals(陈艺彩,谢小保,施庆珊,等. 精细与专用化学品),2010,18(1):43,2010. |
[2] | Yang R J,Wei B W,Yu W J,et al. Chinese Journal of Chro-matography(杨荣静,卫碧文,于文佳,等. 色谱),2011,29 (6):513,2011. |
[3] | Lin F,Mao S L,Chen B,et al. China Leather(林芳,毛树禄,陈斌,等. 中国皮革),2011,40(7):5,2011. |
[4] | Jian L H,Wen H L,Sun J,et al. Chinese Journal of Health Laboratory Technology(简龙海,闻宏亮,孙健,等. 中国卫生检验杂志),2011,21(11):2652,2011. |
[5] | Ministry of Health of the People’s Republic of China. Hygi-enic Standard for Cosmetics. Beijing:Chinese Health Pub-lishing House(中华人民共和国卫生部. 化妆品卫生规范. 北京:中国卫生出版社),2007:234,2007. |
[6] | Feng L,Ying Y,Tan Y,et al. Chinese Journal of Health Laboratory(冯靓,应英,谭莹,等. 中国卫生检验杂志), 2010,20(9):2171,2010. |
[7] | Lin Q B,Wang T J,Song H,et al. Food Additives & Con-taminants:Part A,2010,27(12):1775,2010. |
[8] | Wang T J.【MS Dissertation】. Taiyuan:Shanxi University (王天娇.【硕士学位论文】. 太原:山西大学),2011:35,2011. |
[9] | BS EN 71-11:2005 Safety of Toys:41,2005. |
[10] | Zhang J M,Pan Y N,Bai H. Industrial Water Treatment (张建枚,潘亚男,白桦. 工业水处理),2011,31(5):70,2011. |
[11] | Willingham G L. America Patent,5094957.【1992-03-10】,1992. |
[12] | Geyer W G. America Patent,3975155.【1976-08-17】,1976. |
[13] | Chen Z F,Ying G G,Lai H J,et al. Anal Bioanal Chem, 2012,404(10):3175,2012. |
[14] | Wu T,Wang C,Wang X,et al. Chinese Journal of Analyti-cal Chemistry(武婷,王超,王星,等. 分析化学),2007,35 (10):1439,2007. |
[15] | Li J,Zhao J H. Chinese Journal of Health Laboratory Tech-nology(李洁,赵金辉. 中国卫生检验杂志),2000,10(5):520,2000. |
[16] | HG/T 3657-2008,2008. |
[17] | Gerardo A R,Thierry D,Marta L,et al. J Chromatogr A, 2012,1270:42,2012. |
- 下载量()
- 访问量()
- 您的评分:
-
10%
-
20%
-
30%
-
40%
-
50%