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[采用气相色谱-串联质谱法和液相色谱-串联质谱法同时测定糙米中的农药残留]

[Simultaneous Determination of Pesticide Residues in Brown Rice Using GC-MS/MS and LC-MS/MS].

作者信息

Kokaji Yoshie, Tomizawa Sanae, Kamijo Kyoko, Nakajima Takayuki, Yamamoto Kazuoki, Saito Yuri, Takada Tomomi, Shiradoh Hiroko, Ohsawa Yoshihiro, Oyama Ayane, Noguchi Maiko, Yokoyama Tomoko, Sasamoto Takeo

机构信息

Tokyo Metropolitan Institute of Public Health.

出版信息

Shokuhin Eiseigaku Zasshi. 2023;64(6):246-252. doi: 10.3358/shokueishi.64.246.

Abstract

This study developed a method that simultaneously detected 283 pesticide residues in brown rice using GC-MS/MS and LC-MS/MS. In this method, we examined the desirable amount of sodium chloride required for salting out and the SPE cartridge required for clean-up. Pesticide residues from the sample were extracted with acetonitrile using a homogenizer and mixed with salts including anhydrous magnesium, two types of citrate, and sodium chloride. The sample solution of the acetonitrile layer was cleaned up using the GCB/NH (200 mg/200 mg, 6 mL) SPE cartridge. The determination method was validated using two concentrations (0.01 and 0.1 μg/g) of 283 pesticides based on the validation guideline of the Ministry of Health, Labor and Welfare in Japan. Of the 283 pesticides, 250 were detected satisfactorily. In addition, 59 brown rice samples sold in Tokyo were surveyed using the same method. Out of 44 samples, 12 pesticide residues below MRLs were detected. Therefore, this developed method is useful for the simultaneous determination of pesticide residues in brown rice.

摘要

本研究开发了一种使用气相色谱-串联质谱法(GC-MS/MS)和液相色谱-串联质谱法(LC-MS/MS)同时检测糙米中283种农药残留的方法。在该方法中,我们研究了盐析所需的氯化钠适宜用量以及净化所需的固相萃取柱。样品中的农药残留用乙腈通过匀浆器提取,并与包括无水镁、两种柠檬酸盐和氯化钠在内的盐混合。乙腈层的样品溶液使用GCB/NH(200 mg/200 mg,6 mL)固相萃取柱进行净化。根据日本厚生劳动省的验证指南,使用两种浓度(0.01和0.1 μg/g)的283种农药对测定方法进行了验证。在283种农药中,有250种得到了满意的检测结果。此外,使用相同方法对东京销售的59个糙米样品进行了检测。在44个样品中,检测到12种低于最大残留限量的农药残留。因此,这种开发的方法对于同时测定糙米中的农药残留是有用的。

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