A Study On Analytical Methods Of Irritant Components In Lachrymator

Aerosol defense sprays usually using o-chlorobenzamalononitrile(CS) and nonivamide(OC) as the irritant agent, is the necessary weapon of national police force to maintain social order. The establishment of analytical methods for irritant agents can be used for quality control of aerosol defense sprays, which could ensure the safety and reliability. The main research content of this paper is as follows:Firstly, The method for the determination of CS and OC by UV spectrophotometry was established in this paper. The linear relationship is good in the range of 0.1μg/m L~25μg/m L(CS) and 1μg/mL~200μg/m L(OC) with correlation coefficient of 0.9990, and detection limits were 0.04μg/m L and 0.3μg/mL. The average recovery were 97.37% and 102.51% with the RSD were 1.04% and 0.64% respectively.Secondly, high performance liquid chromatography method was established to detect the irritant components in lachrymator. Through the optimization of chromatography conditions, this paper established the following chromatographic conditions: the mobile phase, which flow rate was 1mL/min, was composed with methanol and water(8:2, V/V). The detection wavelength was 280 nm. This method can be applied to determination of irritant agents in lachrymator. The linear relationship is good in the range of 0.2μg/m L~1000μg/mL(CS), 1μg/mL~1000μg/m L(OC) and 1μg/m L~1000μg/mL(DC), while the detection limits were 0.02μg/mL 、0.05μg/mL and 0.06μg/mL respectively. The average recovery were 100.33%、99.58% and 100.33% with the RSD were 1.61%、1.08% and 2.67% respectively.Then, this paper used gas chromatography to analyze the stimulating components of the lachrymator. The sample solution containing CS、OC or DC, separated on the capillary column HP-5 with N2 as carrier gas at a flow rate of 1m L/min, was detected by a flame ionization detector(FID). Inlet and detector temperatures both were 250℃ with H2(30mL/min), air(300mL/min) and make up gas(N2: 25mL/min). The program of temperature was from 100℃(0.5min) to 250℃ at a rate of 25℃/min. Injection volume was 1μL with the split ratio was 1/10. Relevant validation experiments confirmed that the linear relationship is good in the range of 0.1μg/mL~2500μg/m L(CS), 1μg/mL~1000μg/mL(OC) and 10μg/m L~1000μg/mL(DC), with the detection limits were 0.1μg/mL 、0.3μg/m L and 1μg/m L respectively. The average recovery were 99.32%、94.64% and 97.67% with the RSD were 2.77%、2.73% and 4.9% respectively.Finally, through the comprehensive comparison of these results above, this paper get the conclusion that the high performance liquid chromatography is the most suitable analytical method for the stimulating component detection. This method owning high sensitivity and accuracy, low detection limit, wide linear range, can be applied to detect the irritant agents(CS、OC、DC) in lachrymator.