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RP-HPLC method for the determination o / w type microemulsion Cyhalothrin


Tube, resulting in deactivation of the liner test sample adsorption or decomposition. To solve these problems, the author through many experiments, the establishment of the RP-HPLC to determine Cyhalothrin Microemulsion. [Received】 2008-09-25 【About】 Lam Hing Fat (1979), male, Fujian Zherong, engineers, mainly engaged in pesticide analysis testing. 86 Guangdong Chemical [link widoczny dla zalogowanych] gdchem. corn2009 No. 1 Volume 36, No. 189, Figure 4, the total cyhalothrin UV scan Fig4UVscanabsorptionspectrumoflambda-cyhalothrin2-2 to determine the minimum detection limit of 3 times the signal to noise ratio to determine the minimum detection limit of this method is 1.9x10g , indicating that the method is sensitive,[link widoczny dla zalogowanych], to meet the testing requirements. 2.3 The working curve and the linear relationship in the determination to take the front Cyhalothrin prepared standard solution, respectively,[link widoczny dla zalogowanych], with electronic Continuous pipette Pipette 2,4,6,8,10 mL stock solution in 25mL capacity of 5 bottle, respectively, diluted with methanol to the mark, shake, dubbed the standard solution together with 5 copies of the undiluted standard solution were determined in accordance with the detection method to the measured peak area for the vertical axis, the concentration (gg / mL) for the abscissa to do working curve, the regression equations were:) - 3.228x +145.23, correlation coefficient R = 0.9993. The results showed that: Cyhalothrin in 162.24gg/mL ~ 2028.00gg/mL well within the range, the linear range, shown in Figure 5. Standard solution concentration / (gg'mL) Figure 5 cyhalothrin standard linear graph Fig. 5Thelinearoflambda-cyhalothrin2.4 high-precision test of 32448g/mL cyhalothrin standard solution method for repeated measurements at 5 times (see Table 1), resulting in relative standard deviation of the method is 0.27%, indicating that the precision degree of good. Table 1 The precision of the results of Tab. 1Precisionstest2.5 accuracy for determination of the content has been added in front of the samples were prepared cyhalothrin standard solution 2,4,6,8,10 mL, measured under the above chromatographic conditions were calculated recoveries ( Table 2), measured under these conditions, recoveries were 98.9% ~ 100.5% of the Q, the average recoveries were 99.6%, relative standard deviation was 0.6%. Table 2 The recovery test results Yab. 2Precisionstest2.6 samples for testing than the use of gas chromatography Agilent6890n, with 0.32mmx30ITIiTI, HP a 5 column samples were measured, and the injection port temperature 280 ℃, the column temperature was 240 ℃, detector temperature 280 ℃,[link widoczny dla zalogowanych], carrier gas flow rate 2 .5mL/min,[link widoczny dla zalogowanych], injection volume 1, the internal standard, the Commission octyl phthalate as internal standard. To avoid sample contamination of surface active agent additive decomposition of the liner caused by the sample, the sample preparation process using chloroform extraction, the organic membrane filters, each needle to the sample used to replace the liner activity of the test results to ensure the accuracy, The average test result is 2.69%,[link widoczny dla zalogowanych], determined by RP-HPLC results was 2.68% average relative deviation of 0.4%, with satisfactory results. 3 Conclusions This paper proposes a 2.5% Cyhalothrin Microemulsion phase high performance liquid chromatography, gas chromatography not only overcome the micro-emulsion when the surfactant and cosurfactant contamination caused by sample decomposition liner , but also solve the normal-phase high performance liquid chromatography micro-emulsion problems. The method has high sensitivity and wide linear range, higher accuracy and precision, simple operation, suitable for cyhalothrin micro-emulsion production, quality inspection and other fields.
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