Determination of 60 steroid hormones in sports nutrition foods by ultra performance liquid chromatography-tandem mass spectrometry

doi:10.3724/SP.J.1123.2024.03020

Abstract

Abstract:

Recent societal developments and improving living standards have witnessed a growing enthusiasm for sport and fitness along with a boom in sports nutrition foods. However, rapid industrial development has led to product quality and safety issues becoming increasingly important. Steroid hormones exhibit physiological effects that include promoting protein synthesis, increasing muscle mass, and reducing body fat. Driven by vested interests, some unscrupulous traders illegally add steroid hormones to sports nutrition foods to improve sports performance and relieve muscle pain, which poses a potential threat to human health. Therefore, establishing a method for determining steroid hormones in sports nutrition foods is of great practical importance.

In this study, an analytical method for the simultaneous determination of 60 steroid hormones in sports nutrition foods was developed using QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The MS parameters and chromatographic conditions were optimized for the 60 steroid hormones, and the extraction solvents and purification methods were systematically optimized to facilitate rapid screening and accurate quantitative analysis of these hormones in sports nutrition foods. Samples were extracted with 1.0% formic acid in methanol, partitioned with sodium chloride, and purified using 150 mg of PSA and 150 mg of C₁₈ powder. The clean-up solution was evaporated to near dryness under a stream of nitrogen and the residue was reconstituted with 50% methanol aqueous solution. The 60 target compounds were separated on a Waters Acquity UPLC HSS T₃ column (100 mm×2.1 mm, 1.8 μm) with 0.1% (v/v) formic acid aqueous solution (containing 10 mmol/L ammonium acetate) and methanol as the mobile phases. The analytes were determined by multiple reaction monitoring (MRM) in positive electrospray ionization mode (ESI⁺) and quantified using the external standard method. The method was validated under the optimized conditions, with the 60 steroid hormones found to exhibit good linearities in the 1.0-100 ng/mL range with correlation coefficients (r) greater than 0.99. The limits of detection (LODs) and limits of quantification (LOQs) were 0.2-0.8 μg/kg and 0.6-2.4 μg/kg, respectively. At three spiked levels on whey protein powder (solid), pectin protein peptide (semi-solid) and energy drink (liquid) as blank matrix, the mean recoveries of the 60 steroid hormones were 73.7%-112.7% with relative standard deviations (RSDs) of 3.2%-10.1% (n=6). Thirteen batches of commercially available sports nutrition products were screened using the newly developed method, with five positive samples detected. Progesterone (an endogenous hormone) was detected at levels of 12.6-25.4 μg/kg in four samples of whey protein powder, and boldenone (which is a prohibited drug for athletes) was detected at 14.6 μg/kg in one sports nutrition liquid, confirming that illegal steroid hormones are indeed added to sports nutrition foods; consequently, relevant national departments need to strengthen their monitoring of such substances in such foods. The developed method is simple, efficient, sensitive, reproducible, and suitable for the rapid screening and quantitative analysis of steroid hormones in sports nutrition foods, thereby providing technical support for the daily supervision of steroid hormones in these foods.

Key words: ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), QuEChERS, steroid hormones, sports nutrition food

CLC Number:

O658

CAI Xiaoming, WU Shaoming, YU Qing, HUANG Hehe, ZHENG Qiuping, HE Menghang, DAI Ming, OUYANG Liqun. Determination of 60 steroid hormones in sports nutrition foods by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2024, 42(12): 1173-1188.

Figures/Tables 11

References

[1]	Zhang S, Mo X Q, Zeng Q Y, et al. China Food Safety Magazine, 2023, 28(2): 125
[1]	张斯, 莫锡乾, 曾绮莹, 等. 食品安全导刊, 2023, 28(2): 125
[2]	Plotan M, Elliott C T, Frizzell C, et al. Food Chem, 2014, 159(15): 157
[3]	Guo C, Wang K A. Guizhou Sports Science and Technology, 2020, 5(1): 62
[3]	郭超, 王康安. 贵州体育科技, 2020, 5(1): 62
[4]	Arini L A. IOP Conference Series: Earth Environ Sci, 2021, 913(1): 012085
[5]	Mohammed H A S, Mirdamadi M, Szucs F K, et al. Biochem Pharmacol, 2024, 222: 110632
[6]	Wang Q S, Wang T Y. Chinese Pharmacological Bulletin, 2018, 34(12): 1647
[6]	王琪珊, 王婷玉. 中国药理学通报, 2018, 34(12): 1647
[7]	Yang C Y, Guo L, Yu T E, et al. Biomedical Transformation, 2023, 4(4): 10
[7]	杨春瑛, 郭蕾, 虞铁儿, 等. 生物医学转化, 2023, 4(4): 10
[8]	Dong Y G, Zhang X J, Chen F Z, et al. Chinese Nursing Research, 2019, 33(9): 1457
[8]	董元鸽, 张晓菊, 陈凤珍, 等. 护理研究, 2019, 33(9): 1457
[9]	Zhang Q, Xu C, Tang C K. Progress in Biochemistry and Biophysics, 2022, 49(2): 292
[9]	张强, 许璨, 唐朝克. 生物化学与生物物理进展, 2022, 49(2): 292
[10]	Zou L H. Guangdong Vocational Technical Education and Research 2011, 2(10): 126
[10]	邹丽红. 广东职业技术教育与研究, 2011, 2(10): 126
[11]	Xu D M, Zeng S M, Liu X C, et al. Chinese Journal of Chromatography, 2022, 40(5): 423
[11]	徐敦明, 曾三妹, 柳训才, 等. 色谱, 2022, 40(5): 423
[12]	Chen X P, Gu C Q, Qi Y, et al. Food Science, 2018, 39(8): 314
[12]	陈晓鹏, 顾采琴, 綦艳, 等. 食品科学, 2018, 39(8): 314
[13]	Ministry of Agriculture and Rural Affairs. No. 250 Bulletin of the Ministry and Rural Affairs of the People’s Republic of China. (2019-12-27) [2024-09-02]. https://nyncj.gz.gov.cn/fw/syaqsygd/content/post_6867903.html
[13]	农业农村部. 中华人民共和国农业农村部公告第250号. (2019-12-27)[2024-09-02]. https://nyncj.gz.gov.cn/fw/syaqsygd/content/post_6867903.html
[14]	Silva A C A, Ebrahimi-Najafadabi H, Mcginitie T M, et al. Anal Bioanal Chem, 2015, 407(14): 4091
[15]	Zhou J, Huang Y M, Gong Y F, et al. Chemical Analysis and Meterage, 2016, 25(2): 52
[15]	周江, 黄艳美, 龚越飞, 等. 化学分析计量, 2016, 25(2): 52
[16]	Matraszek-Zuchowska I, Wozniak B, Posyniak A. Food Anal Method, 2017, 10(3): 739
[17]	Wolecki D, Caban M, Pazdro K, et al. Talanta, 2019, 200(6): 316
[18]	Liu H C, Li N, Lin T, et al. Chinese Journal of Chromatography, 2015, 33(11): 1163
[18]	刘宏程, 李宁, 林涛, 等. 色谱, 2015, 33(11): 1163
[19]	Han S Y, Yu H M, Song Y L, et al. Chinese Journal of Chromatography, 2018, 36(3): 285
[19]	韩疏影, 俞慧敏, 宋易霖, 等. 色谱, 2018, 36(3): 285
[20]	Qiu Q L, Chen X H, Pan S D, et al. Chinese Journal of Chromatography, 2022, 40(7): 669
[20]	邱巧丽, 陈晓红, 潘胜东, 等. 色谱, 2022, 40(7): 669
[21]	Ogue N, Kürzinger L, Kendl S, et al. Clin Chem Lab Med, 2024, 62(5):919
[22]	Yin Y, Yu S, Qiu L, et al. J Chromatogr B Anal Technol Biomed Life Sci, 2019, 1113: 84
[23]	Chang Y L, Chen G Y, Lee B C, et al. Hypertens Res, 2023, 8(46): 1983
[24]	Zhu H P, Zhang L, Zhang B Y. Standard & Quality of Light Industry, 2019(1): 53
[24]	朱海佩, 张亮, 张碧宇.轻工标准与质量, 2019(1): 53
[25]	Yang P P, Liu H, Li L X. China Surfactant Detergent & Cosmetics, 2021, 51(5): 468
[25]	杨飘飘, 刘红, 李丽霞. 日用化学工业, 2021, 51(5): 468
[26]	Qiao Y S, Dong Y L, Huang C F, et al. China Surfactant Detergent & Cosmetics, 2021, 51(12): 1259
[26]	乔亚森, 董亚蕾, 黄传峰, 等. 日用化学工业, 2021, 51(12): 1259
[27]	Lv Q F, Peng M, Liang H M, et al. Analytical Instrumentation, 2021, 24(5): 24
[27]	吕琼芳, 彭敏, 梁惠明, 等. 分析仪器, 2021, 24(5): 24
[28]	Yang G Y, Sha L N, Liang Q Y, et al. Chinese Journal of Analysis Laboratory, 2021, 40(8): 959
[28]	杨光勇, 沙丽娜, 梁秋艳, 等. 分析试验室, 2021, 40(8): 959
[29]	Luo H T, Huang X L, Wu H Q, et al. Chinese Journal of Chromatography, 2017, 35(8): 816
[29]	罗辉泰, 黄晓兰, 吴惠勤, 等. 色谱, 2017, 35(8): 816
[30]	Fang C R, Gao J, Wang Y X, et al. Chinese Journal of Chromatography, 2018, 36(11): 1119
[30]	方从容, 高洁, 王雨昕, 等. 色谱, 2018, 36(11): 1119
[31]	Zhao Q R, Liu H, Meng Y P, et al. Chinese Journal of Chromatography, 2023, 41(12): 1084
[31]	赵倩茹, 刘骅, 孟雅萍, 等. 色谱, 2023, 41(12): 1084
[32]	Wu S M, Cai X M, Zhou P, et al. Chinese Journal of Food Science, 2020, 41(16): 320
[32]	吴少明, 蔡小明, 周鹏, 等. 食品科学, 2020, 41(16): 320

No.	Linear equation	r	LODs/(μg/kg)			LOQs/(μg/kg)
No.	Linear equation	r	Whey protein powder	Pectin protein peptide	Energy drink	Whey protein powder	Pectin protein peptide	Energy drink
1	y=2.69×10⁴x+3.40×10⁴	0.997	0.6	0.6	0.3	1.8	1.9	0.9
2	y=1.10×10⁵x+8.86×10⁴	0.993	0.8	0.6	0.4	2.4	1.8	1.2
3	y=2.81×10⁴x+5.80×10⁴	0.990	0.5	0.5	0.5	1.5	1.6	1.4
4	y=1.07×10⁴x+9.31×10⁴	0.997	0.6	0.6	0.5	1.8	1.9	1.5
5	y=8.98×10³x+1.39×10⁴	0.988	0.4	0.4	0.4	1.2	1.3	1.1
6	y=1.87×10⁴x+3.70×10⁵	0.993	0.6	0.6	0.6	1.8	1.9	1.7
7	y=1.17×10⁴x+1.08×10⁴	0.998	0.3	0.3	0.3	0.9	1.0	0.8
8	y=1.09×10⁴x+9.74×10⁴	0.995	0.4	0.4	0.4	1.2	1.3	1.1
9	y=1.66×10⁴x+6.96×10⁴	0.997	0.8	0.6	0.5	2.4	1.8	1.5
10	y=7.17×10⁴x+6.17×10⁴	0.994	0.2	0.2	0.2	0.6	0.6	0.6
11	y=7.61×10⁴x+4.71×10⁴	0.991	0.4	0.4	0.4	1.2	1.3	1.1
12	y=5.01×10⁴x+2.24×10⁴	0.991	0.4	0.4	0.4	1.2	1.3	1.1
13	y=1.77×10⁴x+2.27×10⁴	0.997	0.7	0.5	0.4	2.1	1.5	1.3
14	y=7.82×10⁴x+5.42×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
15	y=2.86×10⁴x+3.18×10⁴	0.996	0.3	0.3	0.3	0.9	1.0	0.8
16	y=7.67×10⁵x+3.41×10⁵	0.999	0.4	0.4	0.4	1.2	1.3	1.1
17	y=6.26×10⁵x+8.36×10⁴	0.995	0.5	0.5	0.5	1.5	1.6	1.4
18	y=3.81×10⁴x+6.41×10⁴	0.996	0.4	0.4	0.4	1.2	1.3	1.1
19	y=9.29×10⁴x+1.09×10⁵	0.993	0.5	0.5	0.5	1.5	1.6	1.4
20	y=1.72×10⁵x+3.52×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
21	y=2.34×10⁴x+1.33×10⁴	0.998	0.7	0.6	0.5	2.1	1.8	1.5
22	y=1.34×10⁵x+1.38×10⁴	0.995	0.6	0.6	0.6	1.8	1.9	1.7
23	y=6.42×10⁴x+6.68×10⁴	0.998	0.4	0.4	0.4	1.2	1.3	1.1
24	y=1.98×10⁴x+1.74×10⁴	0.996	0.6	0.5	0.4	1.8	1.5	1.3
25	y=8.79×10⁴x+1.52×10⁴	0.997	0.6	0.6	0.5	1.8	1.9	1.5
26	y=8.46×10⁴x+4.06×10⁴	0.999	0.6	0.4	0.3	1.8	1.2	1.0
27	y=3.22×10⁴x+1.09×10⁴	0.998	0.6	0.6	0.4	1.8	1.9	1.2
28	y=4.51×10⁴x+4.85×10⁴	0.993	0.5	0.5	0.5	1.5	1.6	1.4
29	y=1.01×10⁴x+3.20×10⁴	0.999	0.4	0.4	0.4	1.2	1.3	1.1
30	y=4.36×10⁴x+1.91×10⁴	0.993	0.6	0.6	0.6	1.8	1.9	1.7
31	y=1.99×10⁴x+2.80×10⁴	0.998	0.7	0.5	0.4	2.1	1.5	1.2
32	y=1.65×10⁴x+2.71×10⁴	0.996	0.5	0.5	0.5	1.5	1.6	1.4
33	y=7.89×10⁴x+1.32×10⁵	0.996	0.4	0.4	0.4	1.2	1.3	1.1
34	y=7.87×10⁴x+1.40×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
35	y=2.00×10⁴x+7.61×10⁴	0.999	0.6	0.6	0.6	1.8	1.9	1.7
36	y=1.07×10⁴x+7.99×10⁴	0.994	0.7	0.5	0.4	2.1	1.5	1.3
37	y=2.36×10⁴x+1.19×10⁴	0.999	0.3	0.3	0.3	0.9	1.0	0.8
38	y=2.38×10⁴x+1.90×10⁴	0.997	0.7	0.6	0.5	2.1	1.8	1.5
39	y=1.01×10⁵x+6.94×10⁴	0.995	0.5	0.5	0.5	1.5	1.6	1.4
40	y=7.42×10⁴x+6.78×10⁴	0.998	0.6	0.6	0.4	1.8	1.9	1.2
41	y=2.06×10⁵x+7.55×10⁴	0.999	0.6	0.6	0.6	1.8	1.9	1.7
42	y=1.01×10⁵x+1.89×10⁴	0.997	0.7	0.5	0.5	2.1	1.5	1.5
43	y=1.51×10⁴x+1.39×10⁵	0.993	0.4	0.4	0.4	1.2	1.3	1.1
44	y=1.59×10⁵x+3.72×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
45	y=5.17×10⁴x+7.31×10⁴	0.992	0.6	0.6	0.6	1.8	1.9	1.7
46	y=4.25×10⁴x+1.51×10⁴	0.998	0.6	0.6	0.6	1.8	1.9	1.7
47	y=4.80×10⁵x+2.48×10⁴	0.999	0.4	0.4	0.4	1.2	1.3	1.1
48	y=8.54×10⁴x+4.71×10⁴	0.999	0.6	0.4	0.3	1.8	1.2	1.0
49	y=5.93×10⁴x-1.17×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
50	y=5.96×10⁵x-2.68×10⁴	0.999	0.7	0.6	0.5	2.1	1.8	1.5
51	y=7.87×10⁴x-4.95×10⁴	0.992	0.4	0.4	0.4	1.2	1.3	1.1
52	y=2.78×10⁴x-1.59×10⁴	0.996	0.6	0.6	0.6	1.8	1.9	1.7
53	y=2.74×10⁴x+2.26×10⁴	0.998	0.5	0.5	0.5	1.5	1.6	1.4
54	y=3.74×10⁴x+6.34×10⁴	0.996	0.6	0.6	0.4	1.8	1.9	1.2
55	y=7.24×10⁴x+1.00×10⁵	0.991	0.6	0.6	0.6	1.8	1.9	1.7
56	y=3.40×10⁴x+1.32×10⁵	0.996	0.8	0.6	0.3	2.4	1.8	0.9
57	y=3.38×10⁵x-3.30×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
58	y=1.56×10⁴x+1.93×10⁴	0.998	0.5	0.5	0.5	1.5	1.6	1.4
59	y=3.27×10⁵x-2.51×10⁴	0.999	0.7	0.5	0.4	2.1	1.5	1.3
60	y=2.24×10⁴x+6.98×10⁴	0.999	0.7	0.6	0.5	2.1	1.8	1.5

No.	Linear equation	r	LODs/(μg/kg)			LOQs/(μg/kg)
No.	Linear equation	r	Whey protein powder	Pectin protein peptide	Energy drink	Whey protein powder	Pectin protein peptide	Energy drink
1	y=2.69×10⁴x+3.40×10⁴	0.997	0.6	0.6	0.3	1.8	1.9	0.9
2	y=1.10×10⁵x+8.86×10⁴	0.993	0.8	0.6	0.4	2.4	1.8	1.2
3	y=2.81×10⁴x+5.80×10⁴	0.990	0.5	0.5	0.5	1.5	1.6	1.4
4	y=1.07×10⁴x+9.31×10⁴	0.997	0.6	0.6	0.5	1.8	1.9	1.5
5	y=8.98×10³x+1.39×10⁴	0.988	0.4	0.4	0.4	1.2	1.3	1.1
6	y=1.87×10⁴x+3.70×10⁵	0.993	0.6	0.6	0.6	1.8	1.9	1.7
7	y=1.17×10⁴x+1.08×10⁴	0.998	0.3	0.3	0.3	0.9	1.0	0.8
8	y=1.09×10⁴x+9.74×10⁴	0.995	0.4	0.4	0.4	1.2	1.3	1.1
9	y=1.66×10⁴x+6.96×10⁴	0.997	0.8	0.6	0.5	2.4	1.8	1.5
10	y=7.17×10⁴x+6.17×10⁴	0.994	0.2	0.2	0.2	0.6	0.6	0.6
11	y=7.61×10⁴x+4.71×10⁴	0.991	0.4	0.4	0.4	1.2	1.3	1.1
12	y=5.01×10⁴x+2.24×10⁴	0.991	0.4	0.4	0.4	1.2	1.3	1.1
13	y=1.77×10⁴x+2.27×10⁴	0.997	0.7	0.5	0.4	2.1	1.5	1.3
14	y=7.82×10⁴x+5.42×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
15	y=2.86×10⁴x+3.18×10⁴	0.996	0.3	0.3	0.3	0.9	1.0	0.8
16	y=7.67×10⁵x+3.41×10⁵	0.999	0.4	0.4	0.4	1.2	1.3	1.1
17	y=6.26×10⁵x+8.36×10⁴	0.995	0.5	0.5	0.5	1.5	1.6	1.4
18	y=3.81×10⁴x+6.41×10⁴	0.996	0.4	0.4	0.4	1.2	1.3	1.1
19	y=9.29×10⁴x+1.09×10⁵	0.993	0.5	0.5	0.5	1.5	1.6	1.4
20	y=1.72×10⁵x+3.52×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
21	y=2.34×10⁴x+1.33×10⁴	0.998	0.7	0.6	0.5	2.1	1.8	1.5
22	y=1.34×10⁵x+1.38×10⁴	0.995	0.6	0.6	0.6	1.8	1.9	1.7
23	y=6.42×10⁴x+6.68×10⁴	0.998	0.4	0.4	0.4	1.2	1.3	1.1
24	y=1.98×10⁴x+1.74×10⁴	0.996	0.6	0.5	0.4	1.8	1.5	1.3
25	y=8.79×10⁴x+1.52×10⁴	0.997	0.6	0.6	0.5	1.8	1.9	1.5
26	y=8.46×10⁴x+4.06×10⁴	0.999	0.6	0.4	0.3	1.8	1.2	1.0
27	y=3.22×10⁴x+1.09×10⁴	0.998	0.6	0.6	0.4	1.8	1.9	1.2
28	y=4.51×10⁴x+4.85×10⁴	0.993	0.5	0.5	0.5	1.5	1.6	1.4
29	y=1.01×10⁴x+3.20×10⁴	0.999	0.4	0.4	0.4	1.2	1.3	1.1
30	y=4.36×10⁴x+1.91×10⁴	0.993	0.6	0.6	0.6	1.8	1.9	1.7
31	y=1.99×10⁴x+2.80×10⁴	0.998	0.7	0.5	0.4	2.1	1.5	1.2
32	y=1.65×10⁴x+2.71×10⁴	0.996	0.5	0.5	0.5	1.5	1.6	1.4
33	y=7.89×10⁴x+1.32×10⁵	0.996	0.4	0.4	0.4	1.2	1.3	1.1
34	y=7.87×10⁴x+1.40×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
35	y=2.00×10⁴x+7.61×10⁴	0.999	0.6	0.6	0.6	1.8	1.9	1.7
36	y=1.07×10⁴x+7.99×10⁴	0.994	0.7	0.5	0.4	2.1	1.5	1.3
37	y=2.36×10⁴x+1.19×10⁴	0.999	0.3	0.3	0.3	0.9	1.0	0.8
38	y=2.38×10⁴x+1.90×10⁴	0.997	0.7	0.6	0.5	2.1	1.8	1.5
39	y=1.01×10⁵x+6.94×10⁴	0.995	0.5	0.5	0.5	1.5	1.6	1.4
40	y=7.42×10⁴x+6.78×10⁴	0.998	0.6	0.6	0.4	1.8	1.9	1.2
41	y=2.06×10⁵x+7.55×10⁴	0.999	0.6	0.6	0.6	1.8	1.9	1.7
42	y=1.01×10⁵x+1.89×10⁴	0.997	0.7	0.5	0.5	2.1	1.5	1.5
43	y=1.51×10⁴x+1.39×10⁵	0.993	0.4	0.4	0.4	1.2	1.3	1.1
44	y=1.59×10⁵x+3.72×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
45	y=5.17×10⁴x+7.31×10⁴	0.992	0.6	0.6	0.6	1.8	1.9	1.7
46	y=4.25×10⁴x+1.51×10⁴	0.998	0.6	0.6	0.6	1.8	1.9	1.7
47	y=4.80×10⁵x+2.48×10⁴	0.999	0.4	0.4	0.4	1.2	1.3	1.1
48	y=8.54×10⁴x+4.71×10⁴	0.999	0.6	0.4	0.3	1.8	1.2	1.0
49	y=5.93×10⁴x-1.17×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
50	y=5.96×10⁵x-2.68×10⁴	0.999	0.7	0.6	0.5	2.1	1.8	1.5
51	y=7.87×10⁴x-4.95×10⁴	0.992	0.4	0.4	0.4	1.2	1.3	1.1
52	y=2.78×10⁴x-1.59×10⁴	0.996	0.6	0.6	0.6	1.8	1.9	1.7
53	y=2.74×10⁴x+2.26×10⁴	0.998	0.5	0.5	0.5	1.5	1.6	1.4
54	y=3.74×10⁴x+6.34×10⁴	0.996	0.6	0.6	0.4	1.8	1.9	1.2
55	y=7.24×10⁴x+1.00×10⁵	0.991	0.6	0.6	0.6	1.8	1.9	1.7
56	y=3.40×10⁴x+1.32×10⁵	0.996	0.8	0.6	0.3	2.4	1.8	0.9
57	y=3.38×10⁵x-3.30×10⁴	0.999	0.5	0.5	0.5	1.5	1.6	1.4
58	y=1.56×10⁴x+1.93×10⁴	0.998	0.5	0.5	0.5	1.5	1.6	1.4
59	y=3.27×10⁵x-2.51×10⁴	0.999	0.7	0.5	0.4	2.1	1.5	1.3
60	y=2.24×10⁴x+6.98×10⁴	0.999	0.7	0.6	0.5	2.1	1.8	1.5

No.	Added/(μg/kg)			Whey protein powder				Pectin protein peptide			Energy drink
No.	Added/(μg/kg)			Recovery/%		RSD/%		Recovery/%		RSD/%	Recovery/%	RSD/%
1		2.50	76.5		6.0		76.8		4.6		78.9		5.8
		5.00	81.3		4.1		86.0		6.6		87.9		4.5
		20.0	84.8		4.8		81.2		6.5		88.7		6.4
2		2.50	91.6		4.5		90.3		5.2		85.1		4.4
		5.00	89.5		4.5		85.6		7.8		93.1		5.1
		20.0	90.4		4.8		90.6		4.8		90.9		4.8
3		2.50	81.5		6.0		82.5		5.2		86.9		4.8
		5.00	85.1		6.2		85.8		6.6		93.5		5.1
		20.0	89.3		4.6		87.9		6.9		86.4		6.4
4		2.50	103.6		7.1		108.2		6.0		102.3		6.8
		5.00	107.8		6.8		97.5		7.7		93.5		4.9
		20.0	101.3		5.6		110.3		7.4		107.8		7.6
5		2.50	84.7		4.2		83.5		6.1		86.0		7.3
		5.00	88.4		5.4		87.1		4.6		86.0		6.0
		20.0	91.4		6.8		90.1		5.8		89.8		4.5
6		2.50	84.1		6.6		84.8		7.4		93.0		5.7
		5.00	87.9		5.5		86.6		7.1		85.4		7.3
		20.0	83.1		6.8		81.9		5.9		89.4		7.0
7		2.50	86.2		7.1		87.5		7.4		84.4		5.8
		5.00	91.1		5.0		89.7		7.7		87.7		7.3
		20.0	87.5		3.2		86.1		5.4		92.5		7.6
8		2.50	83.8		4.2		82.8		3.5		88.9		5.4
		5.00	90.1		5.6		88.8		4.6		85.1		3.5
		20.0	92.5		5.7		85.0		6.1		91.6		4.5
9		2.50	87.6		4.8		86.2		6.2		93.9		6.0
		5.00	92.3		3.2		88.5		5.2		89.0		6.1
		20.0	88.5		7.8		87.2		3.5		93.8		5.1
10		2.50	109.3		6.2		91.4		8.5		103.3		3.5
		5.00	103.5		6.9		107.4		6.9		94.5		8.4
		20.0	106.3		5.4		102.8		7.5		105.7		6.8
11		2.50	86.0		4.8		84.7		5.8		94.4		7.4
		5.00	84.1		6.0		92.4		5.2		87.4		5.7
		20.0	89.5		7.5		88.2		6.6		85.4		5.1
12		2.50	84.1		6.9		82.8		8.1		91.0		6.4
		5.00	86.2		7.1		93.1		7.5		85.4		8.0
		20.0	88.5		6.8		87.2		7.7		87.7		7.4
13		2.50	93.3		5.7		83.1		7.4		89.9		7.6
		5.00	90.3		6.4		89.0		6.2		94.8		7.3
		20.0	86.1		5.1		84.9		7.0		91.7		6.1
14		2.50	92.4		7.1		91.1		5.6		87.6		6.9
		5.00	88.2		4.5		91.3		7.7		93.9		5.5
		20.0	87.4		5.4		86.0		4.8		89.6		7.6
15		2.50	101.2		5.9		99.5		5.8		103.5		4.8
		5.00	93.5		7.9		105.6		6.4		95.3		5.7
		20.0	106.8		6.1		92.1		8.6		104.8		6.3
16		2.50	90.4		6.8		93.5		6.7		88.7		8.5
		5.00	89.5		5.0		88.2		7.4		91.9		6.6
		20.0	93.0		6.2		91.5		5.4		91.0		7.3
17		2.50	84.0		4.5		82.6		6.9		94.4		5.4
		5.00	85.7		7.6		90.4		4.8		85.3		6.8
		20.0	86.3		8.3		85.0		8.2		87.0		4.8
18		2.50	93.4		6.8		89.5		9.0		87.7		8.1
		5.00	88.8		7.5		87.5		7.4		94.9		8.8
		20.0	89.3		3.2		87.9		8.1		90.2		7.3
19		2.50	73.7		7.3		84.3		5.0		79.2		6.4
		5.00	90.2		4.9		86.4		7.1		88.4		4.9
		20.0	86.4		5.8		86.6		4.9		89.1		7.1
20		2.50	104.6		5.4		108.7		5.7		95.3		4.8
		5.00	95.5		5.4		100.3		5.2		92.4		5.6
		20.0	104.5		5.8		105.3		5.2		91.3		5.2
21		2.50	89.1		7.3		90.8		5.7		87.3		5.2
		5.00	92.3		7.5		84.2		7.1		90.4		5.6
		20.0	88.7		5.5		88.4		7.5		86.8		7.1
22		2.50	112.7		8.5		105.2		5.4		91.1		7.4
		5.00	106.4		8.2		100.4		8.4		89.4		5.4
		20.0	104.3		6.8		97.8		8.0		82.7		8.3
23		2.50	88.2		5.0		83.9		6.7		86.4		8.0
		5.00	88.3		6.5		87.5		5.0		86.5		6.6
		20.0	105.7		8.2		90.5		6.3		90.3		4.9
24		2.50	95.4		7.9		85.2		8.0		93.4		6.3
		5.00	87.6		6.7		87.0		7.7		85.8		8.0
		20.0	83.2		8.2		82.3		6.4		89.8		7.6
25		2.50	86.6		8.5		87.9		8.0		84.8		6.4
		5.00	103.6		6.0		90.2		8.4		88.1		8.0
		20.0	94.9		3.9		86.5		5.9		92.9		8.3
26		2.50	91.2		5.0		83.2		3.8		89.3		5.9
		5.00	87.3		6.8		89.2		5.0		104.5		3.9
		20.0	84.4		6.9		85.4		6.7		92.1		4.9
27		2.50	96.3		5.8		86.6		6.8		94.3		6.6
		5.00	88.2		3.9		88.9		5.7		89.4		6.7
		20.0	96.2		9.4		87.6		3.8		94.2		5.6
28		2.50	92.2		7.5		81.1		9.3		90.3		3.9
		5.00	94.2		8.3		88.6		7.5		105.4		6.2
		20.0	89.6		6.5		91.0		8.1		91.4		7.4
29		2.50	86.0		5.8		85.1		6.3		94.8		5.1
		5.00	86.8		7.3		92.8		5.7		87.8		6.3
		20.0	83.3		9.0		88.6		7.1		103.2		5.6
30		2.50	91.1		8.3		83.2		8.8		91.4		7.1
		5.00	88.9		8.5		93.6		8.1		85.8		8.8
		20.0	85.1		8.2		87.6		8.4		88.1		8.1
31		2.50	88.1		6.9		83.5		8.0		90.3		8.3
		5.00	84.6		7.8		89.4		6.8		95.3		8.0
		20.0	88.7		6.2		85.3		7.6		92.2		6.7
32		2.50	87.0		8.5		91.5		6.1		88.0		7.5
		5.00	80.5		5.4		91.8		8.4		94.3		6.0
		20.0	84.1		6.5		86.5		5.2		90.1		5.3
33		2.50	84.2		7.2		85.4		6.3		89.2		5.2
		5.00	87.9		9.5		86.9		7.0		83.6		6.3
		20.0	90.9		7.4		86.4		9.4		85.8		7.0
34		2.50	103.5		8.2		104.6		7.2		108.3		9.3
		5.00	94.5		6.0		93.9		8.0		93.4		7.2
		20.0	107.1		7.5		108.3		5.9		98.2		8.0
35		2.50	85.7		5.4		83.0		7.5		94.8		5.9
		5.00	90.5		9.2		90.8		5.2		85.7		7.4
		20.0	87.0		10.1		85.4		8.9		87.4		5.2
36		2.50	83.3		8.2		89.9		9.8		88.1		8.9
		5.00	89.6		9.0		87.9		8.0		95.4		4.7
		20.0	91.9		3.9		88.4		8.8		90.6		8.0
37		2.50	87.0		6.9		80.1		4.7		75.3		6.1
		5.00	91.7		4.7		82.0		6.8		83.9		4.7
		20.0	88.0		5.5		82.3		4.6		84.7		6.7
38		2.50	89.8		5.1		86.2		5.4		81.2		4.5
		5.00	89.0		5.1		81.7		4.9		88.9		5.3
		20.0	92.4		5.5		80.5		4.9		86.7		5.0
39		2.50	106.5		6.9		96.3		5.4		92.9		5.0
		5.00	98.4		7.2		100.0		6.8		95.9		5.3
		20.0	108.5		5.3		94.9		7.1		92.5		6.7
40		2.50	83.6		8.1		82.3		5.2		86.5		7.0
		5.00	85.7		7.8		81.0		7.9		84.9		5.1
		20.0	88.0		6.4		79.6		7.6		78.5		7.9
41		2.50	92.8		4.8		79.7		6.3		82.0		7.6
		5.00	89.8		6.2		83.1		4.7		82.1		6.3
		20.0	85.6		7.8		86.0		6.0		85.7		4.7
42		2.50	91.8		7.5		81.0		7.6		88.7		6.0
		5.00	87.7		6.3		82.7		7.3		81.5		7.6
		20.0	86.9		7.8		78.2		6.1		85.3		7.3
43		2.50	81.4		8.1		83.5		7.6		80.6		6.1
		5.00	83.6		5.7		85.6		7.9		83.7		7.6
		20.0	86.8		3.7		82.2		5.6		88.3		7.9
44		2.50	89.9		4.8		79.1		3.7		84.8		5.6
		5.00	89.0		6.4		84.7		4.7		81.2		3.7
		20.0	92.4		6.6		81.1		6.3		87.5		4.7
45		2.50	83.5		5.5		82.3		6.4		89.6		6.3
		5.00	85.2		3.7		84.5		5.4		84.9		6.4
		20.0	85.8		9.0		83.2		3.7		89.5		5.3
46		2.50	92.9		7.2		77.1		8.8		85.8		3.7
		5.00	88.3		7.9		84.2		7.1		87.6		8.8
		20.0	88.7		6.2		86.5		7.7		86.8		7.0
47		2.50	79.3		5.5		80.9		6.0		90.1		7.7
		5.00	84.8		6.9		88.2		5.4		83.4		6.0
		20.0	81.2		8.6		84.2		6.8		81.5		5.3
48		2.50	98.3		7.9		79.1		8.4		86.8		6.7
		5.00	89.8		8.1		88.9		7.7		81.5		8.3
		20.0	87.6		7.8		83.2		7.9		83.7		7.7
49		2.50	83.8		6.6		79.3		7.6		85.8		7.9
		5.00	86.8		7.4		84.9		6.4		90.5		7.6
		20.0	83.3		5.8		81.0		7.2		87.5		6.4
50		2.50	107.8		8.1		86.9		5.8		83.6		7.1
		5.00	85.8		5.1		87.2		7.9		89.6		5.7
		20.0	76.6		6.2		82.1		4.9		85.6		7.9
51		2.50	82.9		6.8		81.1		6.0		84.7		5.0
		5.00	83.0		9.1		82.6		6.7		79.4		6.0
		20.0	99.4		7.0		82.0		8.9		81.5		6.6
52		2.50	89.6		7.8		89.3		6.9		84.7		8.9
		5.00	82.3		5.7		84.2		7.6		87.7		6.8
		20.0	78.2		7.2		87.4		5.6		86.8		7.6
53		2.50	81.4		5.1		78.9		7.1		90.1		5.6
		5.00	97.4		8.7		86.3		4.9		81.4		7.0
		20.0	89.2		9.5		81.1		8.5		83.0		5.0
54		2.50	85.7		7.8		85.4		9.3		83.7		8.4
		5.00	82.1		8.6		83.5		7.6		90.6		9.2
		20.0	79.3		3.7		83.9		8.4		86.1		7.6
55		2.50	90.5		6.6		76.0		4.5		89.6		5.8
		5.00	82.9		4.4		77.9		6.4		93.5		4.4
		20.0	90.5		5.2		78.2		4.4		104.8		6.4
56		2.50	86.7		4.9		81.9		5.1		93.6		4.3
		5.00	88.5		4.9		77.6		4.7		102.5		5.0
		20.0	84.3		5.2		76.5		4.7		82.4		4.7
57		2.50	80.8		6.6		82.0		5.1		94.5		4.7
		5.00	81.6		6.8		76.0		6.4		91.3		5.0
		20.0	78.3		5.0		79.7		6.7		88.6		6.4
58		2.50	85.6		7.7		78.2		4.9		82.2		6.7
		5.00	83.6		7.4		77.0		7.6		80.7		4.8
		20.0	80.0		6.1		75.6		7.2		86.5		7.5
59		2.50	82.8		4.5		75.7		6.0		91.4		7.2
		5.00	79.5		5.9		79.0		4.5		85.9		6.0
		20.0	83.4		7.4		81.7		5.7		81.5		4.4
60		2.50	103.4		7.1		87.3		7.2		95.3		5.7
		5.00	89.7		6.0		96.4		6.9		89.4		7.2
		20.0	93.5		7.4		93.1		5.8		97.5		6.9

No.	Added/(μg/kg)			Whey protein powder				Pectin protein peptide			Energy drink
No.	Added/(μg/kg)			Recovery/%		RSD/%		Recovery/%		RSD/%	Recovery/%	RSD/%
1		2.50	76.5		6.0		76.8		4.6		78.9		5.8
		5.00	81.3		4.1		86.0		6.6		87.9		4.5
		20.0	84.8		4.8		81.2		6.5		88.7		6.4
2		2.50	91.6		4.5		90.3		5.2		85.1		4.4
		5.00	89.5		4.5		85.6		7.8		93.1		5.1
		20.0	90.4		4.8		90.6		4.8		90.9		4.8
3		2.50	81.5		6.0		82.5		5.2		86.9		4.8
		5.00	85.1		6.2		85.8		6.6		93.5		5.1
		20.0	89.3		4.6		87.9		6.9		86.4		6.4
4		2.50	103.6		7.1		108.2		6.0		102.3		6.8
		5.00	107.8		6.8		97.5		7.7		93.5		4.9
		20.0	101.3		5.6		110.3		7.4		107.8		7.6
5		2.50	84.7		4.2		83.5		6.1		86.0		7.3
		5.00	88.4		5.4		87.1		4.6		86.0		6.0
		20.0	91.4		6.8		90.1		5.8		89.8		4.5
6		2.50	84.1		6.6		84.8		7.4		93.0		5.7
		5.00	87.9		5.5		86.6		7.1		85.4		7.3
		20.0	83.1		6.8		81.9		5.9		89.4		7.0
7		2.50	86.2		7.1		87.5		7.4		84.4		5.8
		5.00	91.1		5.0		89.7		7.7		87.7		7.3
		20.0	87.5		3.2		86.1		5.4		92.5		7.6
8		2.50	83.8		4.2		82.8		3.5		88.9		5.4
		5.00	90.1		5.6		88.8		4.6		85.1		3.5
		20.0	92.5		5.7		85.0		6.1		91.6		4.5
9		2.50	87.6		4.8		86.2		6.2		93.9		6.0
		5.00	92.3		3.2		88.5		5.2		89.0		6.1
		20.0	88.5		7.8		87.2		3.5		93.8		5.1
10		2.50	109.3		6.2		91.4		8.5		103.3		3.5
		5.00	103.5		6.9		107.4		6.9		94.5		8.4
		20.0	106.3		5.4		102.8		7.5		105.7		6.8
11		2.50	86.0		4.8		84.7		5.8		94.4		7.4
		5.00	84.1		6.0		92.4		5.2		87.4		5.7
		20.0	89.5		7.5		88.2		6.6		85.4		5.1
12		2.50	84.1		6.9		82.8		8.1		91.0		6.4
		5.00	86.2		7.1		93.1		7.5		85.4		8.0
		20.0	88.5		6.8		87.2		7.7		87.7		7.4
13		2.50	93.3		5.7		83.1		7.4		89.9		7.6
		5.00	90.3		6.4		89.0		6.2		94.8		7.3
		20.0	86.1		5.1		84.9		7.0		91.7		6.1
14		2.50	92.4		7.1		91.1		5.6		87.6		6.9
		5.00	88.2		4.5		91.3		7.7		93.9		5.5
		20.0	87.4		5.4		86.0		4.8		89.6		7.6
15		2.50	101.2		5.9		99.5		5.8		103.5		4.8
		5.00	93.5		7.9		105.6		6.4		95.3		5.7
		20.0	106.8		6.1		92.1		8.6		104.8		6.3
16		2.50	90.4		6.8		93.5		6.7		88.7		8.5
		5.00	89.5		5.0		88.2		7.4		91.9		6.6
		20.0	93.0		6.2		91.5		5.4		91.0		7.3
17		2.50	84.0		4.5		82.6		6.9		94.4		5.4
		5.00	85.7		7.6		90.4		4.8		85.3		6.8
		20.0	86.3		8.3		85.0		8.2		87.0		4.8
18		2.50	93.4		6.8		89.5		9.0		87.7		8.1
		5.00	88.8		7.5		87.5		7.4		94.9		8.8
		20.0	89.3		3.2		87.9		8.1		90.2		7.3
19		2.50	73.7		7.3		84.3		5.0		79.2		6.4
		5.00	90.2		4.9		86.4		7.1		88.4		4.9
		20.0	86.4		5.8		86.6		4.9		89.1		7.1
20		2.50	104.6		5.4		108.7		5.7		95.3		4.8
		5.00	95.5		5.4		100.3		5.2		92.4		5.6
		20.0	104.5		5.8		105.3		5.2		91.3		5.2
21		2.50	89.1		7.3		90.8		5.7		87.3		5.2
		5.00	92.3		7.5		84.2		7.1		90.4		5.6
		20.0	88.7		5.5		88.4		7.5		86.8		7.1
22		2.50	112.7		8.5		105.2		5.4		91.1		7.4
		5.00	106.4		8.2		100.4		8.4		89.4		5.4
		20.0	104.3		6.8		97.8		8.0		82.7		8.3
23		2.50	88.2		5.0		83.9		6.7		86.4		8.0
		5.00	88.3		6.5		87.5		5.0		86.5		6.6
		20.0	105.7		8.2		90.5		6.3		90.3		4.9
24		2.50	95.4		7.9		85.2		8.0		93.4		6.3
		5.00	87.6		6.7		87.0		7.7		85.8		8.0
		20.0	83.2		8.2		82.3		6.4		89.8		7.6
25		2.50	86.6		8.5		87.9		8.0		84.8		6.4
		5.00	103.6		6.0		90.2		8.4		88.1		8.0
		20.0	94.9		3.9		86.5		5.9		92.9		8.3
26		2.50	91.2		5.0		83.2		3.8		89.3		5.9
		5.00	87.3		6.8		89.2		5.0		104.5		3.9
		20.0	84.4		6.9		85.4		6.7		92.1		4.9
27		2.50	96.3		5.8		86.6		6.8		94.3		6.6
		5.00	88.2		3.9		88.9		5.7		89.4		6.7
		20.0	96.2		9.4		87.6		3.8		94.2		5.6
28		2.50	92.2		7.5		81.1		9.3		90.3		3.9
		5.00	94.2		8.3		88.6		7.5		105.4		6.2
		20.0	89.6		6.5		91.0		8.1		91.4		7.4
29		2.50	86.0		5.8		85.1		6.3		94.8		5.1
		5.00	86.8		7.3		92.8		5.7		87.8		6.3
		20.0	83.3		9.0		88.6		7.1		103.2		5.6
30		2.50	91.1		8.3		83.2		8.8		91.4		7.1
		5.00	88.9		8.5		93.6		8.1		85.8		8.8
		20.0	85.1		8.2		87.6		8.4		88.1		8.1
31		2.50	88.1		6.9		83.5		8.0		90.3		8.3
		5.00	84.6		7.8		89.4		6.8		95.3		8.0
		20.0	88.7		6.2		85.3		7.6		92.2		6.7
32		2.50	87.0		8.5		91.5		6.1		88.0		7.5
		5.00	80.5		5.4		91.8		8.4		94.3		6.0
		20.0	84.1		6.5		86.5		5.2		90.1		5.3
33		2.50	84.2		7.2		85.4		6.3		89.2		5.2
		5.00	87.9		9.5		86.9		7.0		83.6		6.3
		20.0	90.9		7.4		86.4		9.4		85.8		7.0
34		2.50	103.5		8.2		104.6		7.2		108.3		9.3
		5.00	94.5		6.0		93.9		8.0		93.4		7.2
		20.0	107.1		7.5		108.3		5.9		98.2		8.0
35		2.50	85.7		5.4		83.0		7.5		94.8		5.9
		5.00	90.5		9.2		90.8		5.2		85.7		7.4
		20.0	87.0		10.1		85.4		8.9		87.4		5.2
36		2.50	83.3		8.2		89.9		9.8		88.1		8.9
		5.00	89.6		9.0		87.9		8.0		95.4		4.7
		20.0	91.9		3.9		88.4		8.8		90.6		8.0
37		2.50	87.0		6.9		80.1		4.7		75.3		6.1
		5.00	91.7		4.7		82.0		6.8		83.9		4.7
		20.0	88.0		5.5		82.3		4.6		84.7		6.7
38		2.50	89.8		5.1		86.2		5.4		81.2		4.5
		5.00	89.0		5.1		81.7		4.9		88.9		5.3
		20.0	92.4		5.5		80.5		4.9		86.7		5.0
39		2.50	106.5		6.9		96.3		5.4		92.9		5.0
		5.00	98.4		7.2		100.0		6.8		95.9		5.3
		20.0	108.5		5.3		94.9		7.1		92.5		6.7
40		2.50	83.6		8.1		82.3		5.2		86.5		7.0
		5.00	85.7		7.8		81.0		7.9		84.9		5.1
		20.0	88.0		6.4		79.6		7.6		78.5		7.9
41		2.50	92.8		4.8		79.7		6.3		82.0		7.6
		5.00	89.8		6.2		83.1		4.7		82.1		6.3
		20.0	85.6		7.8		86.0		6.0		85.7		4.7
42		2.50	91.8		7.5		81.0		7.6		88.7		6.0
		5.00	87.7		6.3		82.7		7.3		81.5		7.6
		20.0	86.9		7.8		78.2		6.1		85.3		7.3
43		2.50	81.4		8.1		83.5		7.6		80.6		6.1
		5.00	83.6		5.7		85.6		7.9		83.7		7.6
		20.0	86.8		3.7		82.2		5.6		88.3		7.9
44		2.50	89.9		4.8		79.1		3.7		84.8		5.6
		5.00	89.0		6.4		84.7		4.7		81.2		3.7
		20.0	92.4		6.6		81.1		6.3		87.5		4.7
45		2.50	83.5		5.5		82.3		6.4		89.6		6.3
		5.00	85.2		3.7		84.5		5.4		84.9		6.4
		20.0	85.8		9.0		83.2		3.7		89.5		5.3
46		2.50	92.9		7.2		77.1		8.8		85.8		3.7
		5.00	88.3		7.9		84.2		7.1		87.6		8.8
		20.0	88.7		6.2		86.5		7.7		86.8		7.0
47		2.50	79.3		5.5		80.9		6.0		90.1		7.7
		5.00	84.8		6.9		88.2		5.4		83.4		6.0
		20.0	81.2		8.6		84.2		6.8		81.5		5.3
48		2.50	98.3		7.9		79.1		8.4		86.8		6.7
		5.00	89.8		8.1		88.9		7.7		81.5		8.3
		20.0	87.6		7.8		83.2		7.9		83.7		7.7
49		2.50	83.8		6.6		79.3		7.6		85.8		7.9
		5.00	86.8		7.4		84.9		6.4		90.5		7.6
		20.0	83.3		5.8		81.0		7.2		87.5		6.4
50		2.50	107.8		8.1		86.9		5.8		83.6		7.1
		5.00	85.8		5.1		87.2		7.9		89.6		5.7
		20.0	76.6		6.2		82.1		4.9		85.6		7.9
51		2.50	82.9		6.8		81.1		6.0		84.7		5.0
		5.00	83.0		9.1		82.6		6.7		79.4		6.0
		20.0	99.4		7.0		82.0		8.9		81.5		6.6
52		2.50	89.6		7.8		89.3		6.9		84.7		8.9
		5.00	82.3		5.7		84.2		7.6		87.7		6.8
		20.0	78.2		7.2		87.4		5.6		86.8		7.6
53		2.50	81.4		5.1		78.9		7.1		90.1		5.6
		5.00	97.4		8.7		86.3		4.9		81.4		7.0
		20.0	89.2		9.5		81.1		8.5		83.0		5.0
54		2.50	85.7		7.8		85.4		9.3		83.7		8.4
		5.00	82.1		8.6		83.5		7.6		90.6		9.2
		20.0	79.3		3.7		83.9		8.4		86.1		7.6
55		2.50	90.5		6.6		76.0		4.5		89.6		5.8
		5.00	82.9		4.4		77.9		6.4		93.5		4.4
		20.0	90.5		5.2		78.2		4.4		104.8		6.4
56		2.50	86.7		4.9		81.9		5.1		93.6		4.3
		5.00	88.5		4.9		77.6		4.7		102.5		5.0
		20.0	84.3		5.2		76.5		4.7		82.4		4.7
57		2.50	80.8		6.6		82.0		5.1		94.5		4.7
		5.00	81.6		6.8		76.0		6.4		91.3		5.0
		20.0	78.3		5.0		79.7		6.7		88.6		6.4
58		2.50	85.6		7.7		78.2		4.9		82.2		6.7
		5.00	83.6		7.4		77.0		7.6		80.7		4.8
		20.0	80.0		6.1		75.6		7.2		86.5		7.5
59		2.50	82.8		4.5		75.7		6.0		91.4		7.2
		5.00	79.5		5.9		79.0		4.5		85.9		6.0
		20.0	83.4		7.4		81.7		5.7		81.5		4.4
60		2.50	103.4		7.1		87.3		7.2		95.3		5.7
		5.00	89.7		6.0		96.4		6.9		89.4		7.2
		20.0	93.5		7.4		93.1		5.8		97.5		6.9

Sample	Number of compounds	Analytical method	Preparation method	Preparation time/min	V(Organic solvent)/mL	LOD/ (μg/kg)	Ref.
Bird’s nest	45	UPLC-MS/MS	SPE	>120	40	0.16-2.0	[11]
Milk powder	42	UPLC-MS/MS	QuEChERS	<60	10	0.06-1.5	[12]
Milk	9	UPLC-MS/MS	QuEChERS	<60	10	0.5-10	[18]
Dairy products	6	UPLC-MS/MS	SPE	>120	327	0.05-0.1	[19]
Bullfrogs	9	UPLC-MS/MS	SPE	>120	10	0.5-1.0	[20]
Cosmetics	22	UPLC-MS/MS	SPE	>120	20	0.1-27.4	[24]
Sports nutrition foods	60	UPLC-MS/MS	QuEChERS	<60	10	0.2-0.8	this work