6类茶叶中15种农药残留过程中产生的基质效应研究

陈璐; 李怀平; 王顾希; 唐祥凯; 冯德建; 魏雨婷

6类茶叶中15种农药残留过程中产生的基质效应研究

陈璐^{1, 2,},
李怀平^{1, 2},
王顾希^{1, 2},
唐祥凯^{1, 2, ,},
冯德建^{1, 2},
魏雨婷³

1.
中国测试技术研究院生物研究所，四川　成都　610021
2.
茶叶标准与检测技术四川省重点实验室，四川　成都　610021
3.
西昌市供排水有限责任公司，四川　西昌　615000

基金项目: 四川省重点研发计划项目（2020YFN0003、2020YFN0154）；四川省自然科学基金项目（2022NSFSC1775）

详细信息

作者简介:
陈璐（1991 — ），女，工程师，主要从事食品质量安全研究，E-mail：165374435@qq.com

通讯作者:
唐祥凯（1986 — ），男，硕士研究生，副研究员，主要从事食品质量安全研究，E-mail：460427982@qq.com

中图分类号: TS272
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出版历程
- 收稿日期: 2023-12-19
- 修回日期: 2024-04-19
- 网络出版日期: 2024-07-10

Study on matrix effects in the detection of 15 pesticide residues in 6 types of tea leaves

CHEN Lu^{1, 2
,},
LI Huaiping^{1, 2},
WANG Guxi^{1, 2},
TANG Xiangkai^{1, 2
, ,},
FENG Dejian^{1, 2},
WEI Yuting³

1.
Institute of Biology, National Institute of Measurement and Testing Technology, Chendu, Sichuan　610021, China
2.
Sichuan Provincial Key Laboratory of Tea Standards and Testing Technology, Chendu, Sichuan　610021, China
3.
Xichang Water Supply and Drainage Co., Ltd., Xichang, Sichuan　615000, China

摘要

摘要: 目的对气相色谱-串联质谱法测定6类茶叶中15种农药残留过程中产生的基质效应进行分析，并就日常检测中常见批量样品同时处理时可采用的替代基质进行探讨。方法茶叶样品经QuEChERS前处理，配制质量浓度在0.01～0.32 mg·L⁻¹的溶剂标准曲线和基质标准曲线，经GC-MS/MS测定后计算基质效应。结果 6类茶叶中15种农药检测过程中均产生增强基质效应，其中以增强强基质效应为主，基质效应区间范围1.35%～411.58%，强、中、弱基质效应分别为73.33%、23.33%、3.33%。以红茶为替代基质测定15种农药时，主要以产生增强弱基质效应为主，整体区间范围为|0.62%|～|59.22%|，强中弱基质效应分别为1.33%、14.67%、84.00%；以混合茶叶为代表基质测定15种农药时，主要以产生抑制弱基质效应为主，整体区间范围为|0.09%|～|48.09%|，强中弱基质效应分别为0、13.33%、86.67%。结论茶叶样品基质复杂，在农残检测时使用基质标曲分析可降低基质效应，提高检测结果的准确度。使用混合茶叶样品作为替代基质配制基质标曲对茶叶农残进行定量分析时，可有效提高批量样品的分析效率。
- 气相色谱-串联质谱 /
- 茶叶 /
- 农药残留 /
- 基质效应 /
- 替代基质
Abstract: Objective Matrix effects in detecting 15 pesticide residues in six types of tea using gas chromatography-tandem mass spectrometry (GC-MS/MS) with a sample pretreatment of QuEChERS were analyzed for assay improvement. Methods Tea samples were pretreated with QuEChERS, and solvent and matrix standard curves for the mass concentrations of 0.01-0.32 mg·L⁻¹ prepared. After a GC-MS/MS determination, the matrix effects were calculated. Results Matrix effects were enhanced in the determination that ranged from 1.35-411.58% with the strong, medium, and weak matrix effects of 73.33%, 23.33%, and 3.33%, respectively. When black tea was used as an alternative matrix, they ranged 0.62-59.22% with the strong, medium, and weak matrix effects at 1.33%, 14.67% and 84.00%, respectively. Whereas, when a mixed tea was applied as an alternative matrix, suppressed matrix effects resulted at 0.09-48.09% with the strong, medium, and weak matrix effects at 0, 13.33% and 86.67%. Conclusion The matrix effects in the pesticide residue detection on teas were complex. Application of a matrix standard curve reduced the matrix effects and improved the determination accuracy. By using mixed tea sample as an alternative matrix, the analysis efficiency was significantly enhanced.
- gas chromatography-tandem mass spectrometry /
- tea /
- pesticide residue /
- matrix effect /
- alternative matrix

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图 1 15种农药典型MRM色谱图

1. 敌敌畏；2.甲拌磷；3.五氯硝基苯；4.毒死蜱；5.马拉硫磷； 6.杀螟硫磷；7.甲基异柳磷； 8.水胺硫磷；9.腐霉利；10.杀扑磷； 11.联苯菊酯；12.甲氰菊酯；13.氯菊酯；14.溴氰菊酯；15.苯醚甲环唑。

Figure 1. Typical MRM chromatogram of 15 pesticide residues

1: dichlorvos; 2: phorate; 3: pentachloronitrobenzene; 4: chlorpyrifos; 5: malathion; 6: fenitrothion; 7: isofenphos-methy; 8: isocarbophos; 9: procymidone; 10: methidathion; 11: bifenthrin; 12: fenpropathrin; 13: permethrin; 14: deltamethrin; 15: difenoconazole.

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图 2 以红茶为代表基质矫正后5类茶叶中15种农药检测过程中产生的基质效应占比

Figure 2. Proportion of matrix effects generated in detecting 15 pesticides in 5 types of tea with black tea used as a representative matrix

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图 3 以混合茶为代表基质矫正后6类茶叶中15种农药检测过程中产生的基质效应占比

Figure 3. Proportion of matrix effects generated in detecting 15 pesticides in 6 types of tea with mixed tea used as a representative matrix

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表 1 15种农药名称、CAS号、色谱及质谱参数及定量限

Table 1. Chemical abstract service(CAS) number,GC-MS/MS parameters and limit of quantitation of 15 pesticide residues

序号 No.	目标物 Compound	CAS号 CAS number	保留时间 Retention time/min	母离子 Precursor ions(m/z)	子离子 Product ions(m/z)	碰撞能量 Collision energy/eV	定量限 limit of quantitation/ （mg·kg⁻¹）	线性范围 Linear range/ （mg·kg⁻¹）
1	敌敌畏 Dichlorvos	62-73-7	6.81	109.0	79.0*	5	0.05	0.01~0.32
1	敌敌畏 Dichlorvos	62-73-7	6.81	184.9	93.0	10	0.05	0.01~0.32
2	甲拌磷 Phorate	298-02-2	14.17	260.0	75.0*	5	0.01	0.01~0.32
2	甲拌磷 Phorate	298-02-2	14.17	230.9	128.9	25	0.01	0.01~0.32
3	五氯硝基苯 Pentachloronitrobenzene	82-68-8	15.32	295.0	237.0*	20	0.05	0.01~0.32
3	五氯硝基苯 Pentachloronitrobenzene	82-68-8	15.32	236.9	142.9	30	0.05	0.01~0.32
4	毒死蜱 Chlorpyrifos	2921-88-2	19.73	196.9	169.0*	15	0.05	0.01~0.32
4	毒死蜱 Chlorpyrifos	2921-88-2	19.73	198.9	171.0	15	0.05	0.01~0.32
5	马拉硫磷 Malathion	121-75-5	20.39	126.9	99.0*	5	0.05	0.01~0.32
5	马拉硫磷 Malathion	121-75-5	20.39	172.9	99.0	15	0.05	0.01~0.32
6	杀螟硫磷 Fenitrothion	122-14-5	20.42	277.0	260.0*	5	0.05	0.01~0.32
6	杀螟硫磷 Fenitrothion	122-14-5	20.42	277.0	109	20	0.05	0.01~0.32
7	甲基异柳磷 Isofenphos-methy	99675-03-3	21.44	199.0	121.0*	10	0.01	0.01~0.32
7	甲基异柳磷 Isofenphos-methy	99675-03-3	21.44	241.1	199.1	10	0.01	0.01~0.32
8	水胺硫磷 Isocarbophos	24353-61-5	21.74	135.9	108.0*	15	0.05	0.01~0.32
8	水胺硫磷 Isocarbophos	24353-61-5	21.74	135.9	69.0	30	0.05	0.01~0.32
9	腐霉利 Procymidone	32809-16-8	23.10	96.0	67.1*	10	0.05	0.01~0.32
9	腐霉利 Procymidone	32809-16-8	23.10	96.0	53.1	15	0.05	0.01~0.32
10	杀扑磷 Methidathion	950-37-8	23.11	144.9	85.0*	5	0.05	0.01~0.32
10	杀扑磷 Methidathion	950-37-8	23.11	144.9	58.1	15	0.05	0.01~0.32
11	联苯菊酯 Bifenthrin	82657-04-3	27.35	181.2	165.2*	25	0.05	0.01~0.32
11	联苯菊酯 Bifenthrin	82657-04-3	27.35	181.2	166.2	10	0.05	0.01~0.32
12	甲氰菊酯 Fenpropathrin	39515-41-8	28.34	207.9	181.0*	5	0.05	0.01~0.32
12	甲氰菊酯 Fenpropathrin	39515-41-8	28.34	264.9	210.0	10	0.05	0.01~0.32
13	氯菊酯 Permethrin	51877-74-8	29.97	183.1	168.1*	10	0.05	0.01~0.32
13	氯菊酯 Permethrin	51877-74-8	29.97	183.1	153.0	15	0.05	0.01~0.32
14	溴氰菊酯 Deltamethrin	52918-63-5	33.13	252.9	93.0*	15	0.05	0.01~0.32
14	溴氰菊酯 Deltamethrin	52918-63-5	33.13	250.7	172.0	5	0.05	0.01~0.32
15	苯醚甲环唑 Difenoconazole	119446-68-3	33.25	322.8	264.8*	15	0.05	0.01~0.32
15	苯醚甲环唑 Difenoconazole	119446-68-3	33.25	264.9	202.0	20	0.05	0.01~0.32
定量离子对。 : quantitative ion.

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表 2 6类茶叶中15种农药检测过程中产生的基质效应比较

Table 2. Matrix effects generated in detecting 15 pesticide residues in 6 types of tea

农药名称 Pesticide name	基质效应 ME/%
农药名称 Pesticide name	绿茶 Green tea	红茶 Black tea	花茶 Scented tea	黑茶 Dark tea	白茶 White tea	乌龙茶 Oolong	绝对平均值 Absolute mean
敌敌畏 Dichlorvos	1.35	31.59	8.81	27.06	35.20	38.15	23.69
甲拌磷 Phorate	6.13	43.31	23.75	72.32	56.16	60.19	43.64
五氯硝基苯 Pentachloronitrobenzene	47.35	23.34	45.46	39.95	48.73	60.08	44.15
毒死蜱 Chlorpyrifos	57.39	48.00	56.25	33.78	66.10	75.31	56.14
马拉硫磷 Malathion	101.11	148.50	123.92	154.93	161.75	153.84	140.68
杀螟硫磷 Fenitrothion	112.99	135.59	126.29	145.96	134.13	156.16	135.19
甲基异柳磷 Isofenphos-methy	66.55	44.65	60.34	61.92	64.59	70.01	61.34
水胺硫磷 Isocarbophos	108.10	140.04	115.11	152.66	158.59	178.60	142.18
腐霉利 Procymidone	57.67	34.95	53.11	73.39	55.28	61.84	56.04
杀扑磷 Methidathion	14.51	180.82	58.92	142.15	138.94	104.98	106.72
联苯菊酯 Bifenthrin	39.66	30.69	40.75	50.40	48.68	50.76	43.49
甲氰菊酯 Fenpropathrin	76.60	75.33	81.19	95.37	94.99	88.00	85.25
氯菊酯 Permethrin	85.72	79.55	83.41	110.82	103.12	107.78	95.07
溴氰菊酯 Deltamethrin	269.31	298.67	304.64	394.83	354.78	366.68	331.49
苯醚甲环唑 Difenoconazole	211.21	391.51	279.99	411.58	344.98	381.49	336.79

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表 3 以红茶为代表基质时5类茶叶中15种农药检测过程中产生的基质效应比较

Table 3. Matrix effects generated in detecting 15 pesticides in 5 types of tea with black tea used as a representative matrix

农药名称 Pesticide name	基质效应 ME/%
农药名称 Pesticide name	绿茶 Green tea	花茶 Scented tea	黑茶 Dark tea	白茶 White tea	乌龙茶 Oolong	绝对平均值 Absolute mean
敌敌畏 Dichlorvos	−22.98	−17.31	−3.45	2.75	4.99	10.29
甲拌磷 Phorate	−25.95	−13.65	20.24	8.96	11.78	16.12
五氯硝基苯 Pentachloronitrobenzene	19.47	17.93	13.46	20.58	29.79	20.25
毒死蜱 Chlorpyrifos	6.34	5.58	−9.61	12.23	18.45	10.44
马拉硫磷 Malathion	−19.07	−9.89	2.59	5.33	2.15	7.81
杀螟硫磷 Fenitrothion	−9.59	−3.95	4.40	−0.62	8.73	5.46
甲基异柳磷 Isofenphos-methy	15.14	10.84	11.93	13.78	17.53	13.85
水胺硫磷 Isocarbophos	−13.30	−10.39	5.26	7.73	16.07	10.55
腐霉利 Procymidone	16.83	13.45	28.48	15.07	19.93	18.75
杀扑磷 Methidathion	−59.22	−43.41	−13.77	−14.91	−27.01	31.66
联苯菊酯 Bifenthrin	6.87	7.70	15.09	13.76	15.36	11.75
甲氰菊酯 Fenpropathrin	0.73	3.34	11.43	11.22	7.23	6.79
氯菊酯 Permethrin	3.44	2.15	17.42	13.13	15.73	10.37
溴氰菊酯 Deltamethrin	−7.37	1.50	24.12	14.07	17.06	12.82
苯醚甲环唑 Difenoconazole	−36.68	−22.69	4.08	−9.47	−2.04	14.99

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表 4 以混合茶为代表基质时6类茶叶中15种农药检测过程中产生的基质效应比较

Table 4. Matrix effects generated in detecting 15 pesticides in 6 types of tea with mixed tea used as a representative matrix

农药名称 Pesticide name	基质效应 ME/%
农药名称 Pesticide name	绿茶 Green tea	红茶 Black tea	花茶 Scented tea	黑茶 Dark tea	白茶 White tea	乌龙茶 Oolong	绝对平均值 Absolute mean
敌敌畏 Dichlorvos	−26.54	−4.62	−21.14	−7.91	−2.00	0.13	10.39
甲拌磷 Phorate	−31.54	−7.56	−20.18	11.15	0.73	3.33	12.41
五氯硝基苯 Pentachloronitrobenzene	−4.26	−19.86	−5.49	−9.07	−3.37	4.01	7.68
毒死蜱 Chlorpyrifos	−6.62	−12.19	−7.30	−20.63	−1.45	4.01	8.70
马拉硫磷 Malathion	−18.27	0.98	−9.00	3.60	6.37	3.16	6.90
杀螟硫磷 Fenitrothion	−13.33	−4.13	−7.92	0.09	−4.73	4.24	5.74
甲基异柳磷 Isofenphos-methy	−1.50	−14.45	−5.17	−4.24	−2.66	0.54	4.76
水胺硫磷 Isocarbophos	−28.59	−17.63	−26.18	−13.29	−11.26	−4.39	16.89
腐霉利 Procymidone	−1.23	−15.46	−4.09	8.62	−2.73	1.39	5.59
杀扑磷 Methidathion	−48.09	27.31	−27.95	9.78	8.33	−7.07	21.42
联苯菊酯 Bifenthrin	−6.75	−12.74	−6.03	0.42	−0.73	0.66	4.55
甲氰菊酯 Fenpropathrin	−5.92	−6.60	−3.48	4.08	3.88	0.15	4.02
氯菊酯 Permethrin	−13.88	−16.75	−14.96	−2.25	−5.82	−3.65	9.55
溴氰菊酯 Deltamethrin	−22.58	−16.43	−15.17	3.73	−4.66	−2.17	10.79
苯醚甲环唑 Difenoconazole	−29.29	11.68	−13.66	16.24	1.11	9.40	13.56

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表 5 添加水平为0.10 mg·kg⁻¹时4种农药在两种定量方式下的平均回收率（n=6）

Table 5. Average recovery rates of 4 pesticides under two quantitative methods at an addition level of 0.10 mg·kg⁻¹（n=6）

茶叶种类 Tea types	标液类型 Standard liquid type	马拉硫磷 Malathion		水胺硫磷 Isocarbophos		溴氰菊酯 Deltamethrin		苯醚甲环唑 Difenoconazole
茶叶种类 Tea types	标液类型 Standard liquid type	平均回收率 Average recovery rate/%	相对标准偏差 RSD/%	平均回收率 Average recovery rate/%	相对标准偏差 RSD/%	平均回收率 Average recovery rate/%	相对标准偏差 RSD/%	平均回收率 Average recovery rate/%	相对标准偏差 RSD/%
绿茶 Green tea	绿茶基质标 Green tea substrate	114.99	3.18	114.84	2.14	112.75	2.16	109.71	2.14
绿茶 Green tea	混合茶基质标 Mixed tea substrate	107.76	4.11	96.41	2.46	93.09	1.63	105.14	3.93
花茶 Scented tea	花茶基质标 Scented tea substrate	90.47	3.46	101.03	1.57	85.54	4.95	89.7	2.46
花茶 Scented tea	混合茶基质标 Mixed tea substrate	91.9	2.51	94.55	1.83	90.55	3.10	89.77	2.68
红茶 Black tea	红茶基质标 Black tea substrate	76.57	3.10	104.14	4.71	87.78	3.33	79.19	4.31
红茶 Black tea	混合茶基质标 Mixed tea substrate	85.24	4.84	102.04	2.97	91.25	4.83	85.29	5.61
黑茶 Dark tea	黑茶基质标 Dark tea substrate	84.03	2.56	106.34	3.79	80.54	2.96	96.53	1.83
黑茶 Dark tea	混合茶基质标 Mixed tea substrate	94.83	2.85	101.44	2.11	87.11	2.49	99.48	3.11
白茶 White tea	白茶基质标 White tea substrate	78.88	3.62	98.74	3.82	107.18	5.10	85.81	4.34
白茶 White tea	混合茶基质标 Mixed tea substrate	80.58	5.12	104.62	4.15	105.03	2.61	88.65	2.77
乌龙茶 Oolong	乌龙茶基质标 Oolong substrate	86.46	3.94	107.9	3.21	80.18	2.27	75.81	3.27
乌龙茶 Oolong	混合茶基质标 Mixed tea substrate	88.6	3.81	108.47	4.19	83.23	3.15	86.41	2.68

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