SPE-GC-MS检测儿童驱蚊扣中8种菊酯类物质

doi:10.3969/j.issn.1001-1803.2020.10.013

摘要/Abstract

摘要：

建立检测市场上儿童驱蚊扣产品中菊酯类物质的气相色谱质谱方法,方法确定了甲醇为萃取溶剂,萃取液经HLB固相萃取小柱净化,以乙酸乙酯为洗脱溶剂,收集洗脱液,洗脱液经旋转蒸发浓缩后,用质谱检测器检测,确定每种菊酯类物质的特征离子,采用选择离子扫描（SIM）,外标法定量。结果表明8种菊酯类化合物的质量浓度在0.05~1.0 mg/L范围内与其对应的峰面积成良好的线性关系,相关系数均不小于0.998,检出限为0.01~0.61 μg/L。3个加标水平样品的平均回收率为91.8%~119.2%,测定结果的相对标准偏差为0.94%~6.43%（n=5）。该方法前处理简便,线性和重复性良好,可用于驱蚊扣产品中菊酯类物质的检测。

关键词: 固相微萃取, 驱蚊扣, 菊酯类, 气相色谱质谱联用仪

Abstract:

A gas chromatography-mass spectrometry （GC-MS） method was developed for the determination of pyrethroids residues in mosquito repellent products for children on the market. Methanol was identified as the extraction solvent. The extraction solution was purified by HLB solid phase extraction column. Ethyl acetate was used as the eluting solvent., After the eluate was concentrated by rotary evaporation, it was detected by a mass spectrometer to determine the characteristic ions of each pyrethroid substance, and quantified by selective ion scanning （SIM） and external standard method. The results show that there is a good linear relationship between the mass concentration of the eight pyrethroids and their corresponding peak area within the range of 0.05-1.0 mg/L,the correlation coefficients are not less than 0.998, and the detection limits are 0.01-0.61 μg/L. The average recoveries of the three spiked level samples are 91.8%-119.2%, and the relative standard deviations are 0.94%-6.43% （n=5）. The method has the advantages of simple pretreatment, good linearity and repeatability, and can be used to detect pyrethroids in mosquito repellent products.

Key words: solid-phase extraction, mosquito repellent products, pyrethroids, GC-MS

中图分类号:

TQ658

谭丽君,李欣. SPE-GC-MS检测儿童驱蚊扣中8种菊酯类物质[J]. 日用化学工业, 2020, 50(10): 731-734.

TAN Li-jun,LI Xin. Determination of eight pyrethroids in children’s mosquito repellent products by SPE-GC-MS[J]. China Surfactant Detergent & Cosmetics, 2020, 50(10): 731-734.

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参考文献 17

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序号	化合物名称	保留时间/min	CAS号	定性离子（m/z）							定量离子（m/z）
1	氟氯菊酯	17.44	82657-04-3	181	,	166					181
2	甲氰菊酯	17.67	64257-84-7	181	,	97	,	125	,	152	181
3	高效氯氟氰菊酯Ⅰ	18.44	91465-08-6	197	,	181	,	141	,	161	197
3	高效氯氟氰菊酯Ⅱ	18.66	76703-62-3	197	,	181	,	141	,	161	197
4	氯菊酯Ⅰ	19.73	52645-53-1	183	,	165	,	91	,	127	183
4	氯菊酯Ⅱ	19.92	61949-77-7	183	,	165	,	91	,	127	183
5	氯氰菊酯Ⅰ	20.13	52315-07-8	181	,	127	,	91	,	163	127
5	氯氰菊酯Ⅱ	20.33	71697-59-1	181	,	127	,	91	,	163	127
6	氟氯氰菊酯Ⅰ	20.42	68359-37-5	181	,	127	,	91	,	163	181
6	氟氯氰菊酯Ⅱ	20.51	83855-46-3	181	,	127	,	91	,	163	181
7	氰戊菊酯Ⅰ	22.17	51630-58-1	125	,	225	,	167	,	152	125
7	氰戊菊酯Ⅱ	22.47	67614-33-9	125	,	225	,	167	,	152	125
8	溴氰菊酯	23.62	52820-00-5	181	,	174	,	93	,	152	174

序号	化合物名称	回归方程	相关系数R²	线性范围/（mg·L^-1）	检出限/（μg·L^-1）	定量限/（μg·L^-1）
1	氟氯菊酯	y=3.444×10⁷x-8.521×10⁵	0. 998 3	0.05~1.0	0.01	0.03
2	甲氰菊酯	y=7.176×10⁶x-1.029×10⁵	0. 998 8	0.05~1.0	0.21	0.63
3	高效氯氟氰菊酯	y=8.662×10⁶x-1.301×10⁵	0. 999 6	0.05~1.0	0.30	0.90
4	氯菊酯	y=2.573×10⁷x-6.658×10⁵	0. 999 1	0.05~1.0	0.16	0.48
5	氯氰菊酯	y=4.390×10⁶x-1.031×10⁵	0. 999 5	0.05~1.0	0.61	1.83
6	氟氯氰菊酯	y=1.920×10⁶x-3.305×10⁴	0. 999 5	0.05~1.0	0.57	1.67
7	氰戊菊酯	y=2.306×10⁷x-5.550×10⁵	0. 999 5	0.05~1.0	0.18	0.54
8	溴氰菊酯	y=1.522×10⁶x-4.220×10⁵	0. 999 4	0.05~1.0	0.18	0.54

序号	化合物名称	回收率/%			RSD/%
序号	化合物名称	0. 1 mg·L^-1	0. 5 mg·L^-1	1. 0 mg·L^-1	0. 1 mg·L^-1	0. 5 mg·L^-1	1. 0 mg·L^-1
1	氟氯菊酯	105.8	103.2	95.4	2.44	3.51	5.12
2	甲氰菊酯	107.8	102.5	119.2	2.92	1.13	4.02
3	高效氯氟氰菊酯Ⅰ	95.4	101.0	101.0	2.01	2.55	3.96
4	高效氯氟氰菊酯Ⅱ	119.2	101.8	116.5	2.68	2.88	4.56
5	氯氰菊酯Ⅰ	101.0	91.8	120.2	2.78	1.66	4.81
6	氯氰菊酯Ⅱ	116.5	97.5	99.0	1.87	2.58	3.76
7	氟氯氰菊酯Ⅰ	120.2	106.0	93.0	3.25	2.88	2.85
8	氟氯氰菊酯Ⅱ	93.0	95.5	111.8	3.73	1.69	4.95
9	氯菊酯Ⅰ	96.4	116.7	95.4	0.94	2.50	5.01
10	氯菊酯Ⅱ	98.5	97.5	100.6	4.48	2.68	2.56
11	氰戊菊酯Ⅰ	94.1	106.0	102.5	6.43	3.51	2.87
12	氰戊菊酯Ⅱ	95.1	95.5	103.2	3.44	1.13	5.12
13	溴氰菊酯	97.0	116.7	99.0	4.92	2.55	5.23